CN109913197B - Oil displacement proppant and preparation method thereof - Google Patents
Oil displacement proppant and preparation method thereof Download PDFInfo
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- CN109913197B CN109913197B CN201910217496.0A CN201910217496A CN109913197B CN 109913197 B CN109913197 B CN 109913197B CN 201910217496 A CN201910217496 A CN 201910217496A CN 109913197 B CN109913197 B CN 109913197B
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Abstract
The invention provides an oil displacement proppant and a preparation method thereof. The apparent density of the oil displacement proppant is 1.00-1.08g/cm3The bulk density is 0.40-0.50g/cm3The proppant comprises the following raw material components by taking the total weight of the raw material components of the proppant as 100 percent: 40-55% of chemically modified first powder material, 20-33% of chemically modified second powder material, 15-20% of prepolymer of thermosetting resin adhesive, 2-4% of organic solvent, 0.1-2% of pore-forming agent and 0.1-2% of oil-displacing agent. The technical scheme provided by the invention is simple and convenient, and easy for industrial production, the effective oil displacement volume ratio of the prepared oil displacement proppant is more than or equal to 1000, and the interfacial tension of produced water containing the oil displacement agent is less than 0.1mN/m, so that the two requirements of oil reservoir fracture support and oil displacement can be met simultaneously.
Description
Technical Field
The invention relates to an oil displacement proppant and a preparation method thereof, belonging to the fields of hydraulic fracturing technology and oil well water injection development.
Background
The hydraulic fracturing transformation is one of core technologies for economic and effective development of low-permeability and ultra-low-permeability and unconventional oil and gas fields, and plays an irreplaceable important role in stable-yield and high-yield development of old oil and gas fields.
The proppant is one of key materials for ensuring high conductivity of the hydraulic fracture, so that the efficient filling of the proppant in the fracture is very important for ensuring the fracturing effect. The apparent density of the conventional proppant quartz sand ceramsite currently used is 2.6-3.9g/cm3And high-viscosity fracturing fluid is required to be carried and transported, so that the reservoir damage is easily caused, and the damage rate is generally between 20 and 60. When the viscosity of the fracturing fluid is low, the conventional high-density proppant is difficult to convey, is easy to settle in the fracture, and has small effective supporting area of the fracture. In contrast, ultra low density proppants are as low as 1.05-1.3g/cm due to density3The minimum flow speed required by suspension transportation is kept one order of magnitude lower than that of the conventional propping agent, so that the transportation and filling efficiency is high, the effective supporting area of the fracture is large, the damage to the reservoir and the artificial fracture is obviously reduced, the damage to the reservoir can be obviously reduced, and the flow conductivity of the fracture is favorably improved.
On the other hand, in the later stage of oil well development, water injection and oil displacement are the most common production tasks, only the water injection effect is poor, and an oil displacement agent needs to be added into water to improve the oil displacement effect. However, because the oil reservoir is heterogeneous, water containing the oil displacement agent can be preferentially discharged from high-permeability large pores and cannot enter low-permeability small pores which need oil displacement as much as possible. Therefore, the oil displacement agent cannot fully exert the oil displacement effect, waste is generated, and oil displacement operation needs to be carried out for many times in a certain period, or the injection pressure of water injection for oil displacement is increased, which are not beneficial to cost reduction and efficiency improvement.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide an oil displacement proppant and a preparation method thereof. The oil displacement proppant is an ultra-low density proppant, can keep basic suspension in clear water or slick water, can be carried and laid by the clear water or slick water, can play an oil displacement function in a larger range, has a higher effective oil removal volume ratio, and can simultaneously meet two requirements of oil reservoir fracture support and oil displacement.
In order to achieve the aim, the invention provides an oil displacement proppant, and the apparent density of the oil displacement proppant is 1.00-1.08g/cm3The bulk density is 0.40-0.50g/cm3The raw materials of the oil displacement proppant comprise a prepolymer of a thermosetting resin adhesive, an organic solvent, a chemically modified mixed powder material, a pore-forming agent and an oil displacement agent;
the chemically modified mixed powder material comprises a chemically modified first powder material and a chemically modified second powder material.
The oil displacement proppant comprises, by taking the total weight of raw materials of the oil displacement proppant as 100%, 40-55% of the first chemically modified powder material, 20-33% of the second chemically modified powder material, 15-20% of a prepolymer of a thermosetting resin adhesive, 2-4% of an organic solvent, 0.1-2% of a pore-forming agent and 0.1-2% of an oil displacement agent.
In the oil-displacing proppant, preferably, the apparent density of the first powder material before chemical modification is 0.35-0.70g/cm3The particle size distribution range before chemical modification is 5-45 μm; more preferably, the median particle diameter D before chemical modification50And 24 μm.
In the oil-displacing proppant, preferably, the apparent density of the second powder material before chemical modification is 2.30-3.90g/cm3The particle size distribution range before chemical modification is 1-6 μm; median particle diameter D before chemical modification50And was 4 μm.
In the oil-displacing proppant, preferably, the heat-resistant temperature of the first powder material before chemical modification is more than or equal to 500 ℃, and the compressive strength of the first powder material before chemical modification is 83-110 MPa.
In the oil-displacing proppant, preferably, the heat-resistant temperature of the second powder material before chemical modification is more than or equal to 500 ℃, and the compressive strength of the second powder material before chemical modification is not lower than that of the first powder material.
In the oil-displacing proppant, preferably, the chemically modified first powder material includes chemically modified fly ash and/or chemically modified hollow glass microspheres.
In the oil displacement proppant, preferably, the chemically modified second powder material comprises chemically modified silica powder and/or chemically modified bauxite.
In the oil displacement proppant, preferably, when the first powder material and the second powder material are chemically modified, the used modifier comprises a diselenide compound; more preferably, the diselenide compound comprises 1, 2-di-n-hexyl diselenide and/or 1, 2-di-n-decyl diselenide.
In the oil-displacing proppant, preferably, when the first powder material and the second powder material are chemically modified, the ratio of the weight of the modifier to the total weight of the chemically modified mixed powder material is 1:200-1: 20; wherein the total weight of the chemically modified mixed powder material is the sum of the weights of the chemically modified first powder material and the chemically modified second powder material.
When inorganic mineral materials (such as kaolin, montmorillonite, attapulgite, hollow glass microspheres, fly ash, silica micropowder and bauxite) are compounded with organic polymer materials, the inorganic mineral materials are difficult to be effectively compounded with the organic polymer materials due to the difference of oleophylic and hydrophilic properties, and a high-performance proppant product is difficult to be prepared. The invention can effectively solve the problems by using the mixed powder material which is chemically modified.
In a preferred scheme of the invention, powder modification is carried out by using a chemical agent comprising a diselenide compound (such as 1, 2-di-n-hexyl diselenide and/or 1, 2-di-n-decyl diselenide), so that lipophilic modification on inorganic mineral materials can be effectively realized, and the structure of the inorganic mineral materials can be protected and higher strength can be kept. When the inorganic mineral material is subjected to oleophylic modification, a commonly used modifying agent such as a silane coupling agent and/or a titanate coupling agent and/or an organic aldehyde compound needs to be modified by using a modifying agent after etching the inorganic mineral material by using strong acid or strong base if the inorganic mineral material is to be effectively modified, but the strong acid or strong base etching can damage the structure of the low-inorganic mineral material and reduce the strength of the low-inorganic mineral material. When the diselenide compound is adopted for modification, the structures of the hollow glass microspheres and the coal ash powder are not obviously damaged, the risk can be effectively avoided, the compressive strength of the proppant is obviously improved, and the proppant with higher strength and better performance is more favorably obtained. In the oil displacement proppant, preferably, the oil displacement agent satisfies the following conditions: after the crude oil/formation water interfacial tension is endured for 24 hours at the temperature of more than 200 ℃, the crude oil/formation water interfacial tension can still be reduced to less than 0.1 mN/m.
In the oil displacement propping agent, preferably, the prepolymer of the thermosetting resin adhesive is in a liquid state, and the viscosity of the prepolymer at 25 ℃ is 500-6000mPa & s; more preferably, the prepolymer of the thermosetting resin adhesive comprises one or a combination of two or more of a prepolymer of a thermosetting epoxy resin, a prepolymer of a thermosetting phenol resin and a prepolymer of a thermosetting polyurethane resin. In the technical scheme provided by the invention, the prepolymer of the thermosetting resin adhesive is preferably cured at the temperature of 150 ℃ and 200 ℃ for 5-30 minutes to obtain a product with the softening point higher than 180 ℃.
In the above flooding proppant, preferably, the organic solvent includes one or a combination of two or more of methanol, ethanol, and acetone.
In the oil displacement proppant, the pore-forming agent preferably comprises dipropyl phthalate, or cetyl alcohol, or xylene, or a combination of two or more of the two. In the above proppant, preferably, the particle size of the proppant is 20 to 200 mesh. The particle size of the proppant can be 20-40 meshes, 40-70 meshes, 70-100 meshes or 100-200 meshes.
In the oil displacement agent proppant, the pore-forming agent is added to provide a channel for the oil displacement agent to be released from the surface layer of the proppant to formation fluid.
The oil displacement proppant is preferably prepared by the following preparation method of the oil displacement proppant.
The invention also provides a preparation method of the oil displacement proppant, which comprises the following steps:
adding a first part of mixture of thermosetting resin adhesive and organic solvent into the chemically modified mixed powder material, and performing adhesion granulation;
adding a mixture obtained by mixing a second mixture of thermosetting resin adhesive and organic solvent with an oil displacement agent and a pore-forming agent at the later stage of the bonding and granulating process to obtain particles;
drying, solidifying, cooling and sieving the particles to obtain the oil displacement proppant;
wherein the weight ratio of the mixture of the first part of thermosetting resin adhesive and the organic solvent to the mixture of the second part of thermosetting resin adhesive and the organic solvent is 97:3-85: 15.
In the above preparation method, preferably, the chemically modified mixed powder material is prepared by a modification method comprising the steps of:
uniformly mixing the first powder material and the second powder material to obtain a mixed powder material;
adding a modifier into the mixed powder material, and then activating at a preset temperature and a preset time to obtain a chemically modified mixed powder material (the material is dried in the activation process, so that the obtained chemically modified mixed powder material is a dried mixed powder material).
In the above modification method, preferably, the predetermined temperature is 60 to 120 ℃, more preferably, 60 to 100 ℃, and further preferably, 70 to 90 ℃.
In the above modification method, preferably, the predetermined time is 1 to 6 hours, more preferably, the predetermined time is 1 to 4 hours, and further preferably, the predetermined time is 2 to 3 hours.
In the above modification method, preferably, when the modifier is added to the mixed powder material, the mixed powder material is in a stirring state, the stirring speed is 900-.
In the above preparation method, preferably, when the particles are dried, the drying temperature is 60 to 100 ℃, and the drying time is 10 to 30 minutes; more preferably, the drying is carried out at a temperature of 80-100 ℃ for a time of 20-30 minutes.
In the above preparation method, preferably, the curing temperature is 150-; more preferably, the curing temperature is 180-200 ℃, and the curing time is 5-15 minutes.
In the above method, preferably, the total time of the binder granulation is 5 to 15 minutes; more preferably, the total time of the adhesive granulation is 8 to 12 minutes, wherein the adhesive granulation time is 6 to 10 minutes before adding a mixture obtained by mixing the mixture of the second thermosetting resin binder and the organic solvent with the oil displacement agent and the pore-forming agent, and the adhesive granulation time is 2 to 3 minutes after adding a mixture obtained by mixing the mixture of the second thermosetting resin binder and the organic solvent with the oil displacement agent and the pore-forming agent.
In the above preparation method, preferably, when the first part of the mixture of the thermosetting resin binder and the organic solvent is added to the chemically modified mixed powder material, the chemically modified mixed powder material is stirred at a stirring speed of 1200-6000 rpm, and the first part of the mixture of the thermosetting resin binder and the organic solvent is added in portions (for example, but not limited to, 10 portions); more preferably, when the first part of the mixture of the thermosetting resin binder and the organic solvent is added to the chemically modified mixed powder material, the chemically modified mixed powder material is stirred at a stirring speed of 1200-5500 rpm, and the first part of the mixture of the thermosetting resin binder and the organic solvent is added in portions (for example, but not limited to, 10 portions).
In the above preparation method, preferably, when the mixture obtained by mixing the second mixture of the thermosetting resin binder and the organic solvent with the oil displacement agent and the pore-forming agent is added in the later stage of the adhesion granulation process, the rotation speed of the mixture in the later stage of the adhesion granulation process is 4500-5500 rpm, and the mixture obtained by mixing the second mixture of the thermosetting resin binder and the organic solvent with the oil displacement agent and the pore-forming agent is added in portions (for example, but not limited to, 10 portions).
In the above preparation method, preferably, in the course of adhesive granulation before adding the mixture obtained after mixing the mixture of the second part of thermosetting resin binder and organic solvent with the oil displacement agent and the pore-forming agent, the stirring speed of the adhesive granulation is 1500-.
In the above preparation method, preferably, in the course of adhesion granulation after adding the mixture obtained by mixing the mixture of the second part of thermosetting resin binder and organic solvent with the oil displacement agent and the pore-forming agent, the stirring speed of the adhesion granulation is 4800-.
In the above preparation method, the granulating equipment may be a granulator.
In the preparation method, the sum of the mass of the mixture of the first part of thermosetting resin adhesive and the organic solvent and the mass of the mixture of the second part of thermosetting resin adhesive and the organic solvent is the sum of the mass of the thermosetting resin adhesive and the organic solvent in the raw oil-displacing proppant component; wherein the sum of the mass of the thermosetting resin binder in the mixture of the first part of thermosetting resin binder and the organic solvent and the mass of the thermosetting resin binder in the mixture of the second part of thermosetting resin binder and the organic solvent is the total mass of the thermosetting resin binders in the oil-displacing proppant raw material component, and the sum of the mass of the organic solvent in the mixture of the first part of thermosetting resin binder and the organic solvent and the mass of the organic solvent in the mixture of the second part of thermosetting resin binder and the organic solvent is the total mass of the organic solvent in the oil-displacing proppant raw material component.
In one embodiment, the preparation method of the flooding proppant comprises the following steps:
putting the first powder material and the second powder material into a granulator, and uniformly stirring at the speed of 600-;
adding a modifier into the mixed powder material, uniformly mixing, and activating at 60-120 ℃ for 1-6 hours to obtain a chemically modified mixed powder material (the material is dried in the activating process, so that the obtained chemically modified mixed powder material is a dried mixed powder material);
putting the chemically modified mixed powder material into a granulator, and uniformly stirring at the speed of 1200-3600 r/min;
dividing a mixture of the thermosetting resin adhesive and the organic solvent obtained by mixing the prepolymer of the thermosetting resin adhesive and the organic solvent into two parts, wherein the weight ratio of the first part to the second part is 97:3-85:15, and uniformly mixing the mixture of the thermosetting resin adhesive and the organic solvent with a pore-foaming agent and an oil-displacing agent to obtain a mixture of the thermosetting resin adhesive and the organic solvent and the pore-foaming agent and the oil-displacing agent;
adding a first part of the mixture of the thermosetting resin binder and the organic solvent into the granulator in batches (such as but not limited to 10 batches), and increasing the stirring speed of the granulator to 3000-6000 rpm for adhesive granulation;
at the later stage of granulation, adding a second mixture of thermosetting resin binder and organic solvent, pore-forming agent and oil displacement agent in batches (such as but not limited to 10 batches), and continuing granulation for a period of time to obtain granules;
and drying, solidifying, cooling and sieving the particles to obtain the proppant.
In the above embodiment, the chemically modified mixed powder material is preferably fed into a granulator and stirred uniformly at a speed of 2500-.
Compared with the prior art, the invention has the following beneficial effects:
(1) the technical scheme provided by the invention has the advantages of simple preparation method, easy operation and strong repeatability, and is suitable for large-scale industrial production.
(2) The oil-displacing proppant provided by the invention has apparent density of 1.00-1.08g/cm3The bulk density is 0.40-0.50g/cm3The oil-displacing proppant may be maintained in basic suspension in clear water or slick water, so that clear water or slick water may be usedThe water is carried and laid, the laying height and length in the cracks are large, and the oil displacement function can be exerted in a larger range. In the preferable scheme of the invention, the particle size distribution of the oil displacement proppant provided by the invention is 20-200 meshes, so that the oil displacement proppant is more beneficial to field application.
(3) The effective oil displacement volume ratio (volume of produced water containing an oil displacement agent/volume of the oil displacement proppant, Vwater/Vpropant) of the oil displacement proppant provided by the invention is more than or equal to 1000, and the interfacial tension of the produced water containing the oil displacement agent is less than 0.1 mN/m.
(4) The oil-displacing proppant provided by the invention has a long-term working temperature of more than or equal to 160 ℃, can meet the requirements of fracturing clear water or slickwater fracturing construction of deep high-temperature oil and gas wells, has low breaking rate under the closed pressure of 10-60MPa, and is beneficial to maintaining higher flow conductivity of a proppant filling layer.
(5) The oil displacement proppant provided by the invention can simultaneously meet two requirements of oil reservoir fracture support and oil displacement. At present, the fracturing construction does not have the requirement on oil displacement, so materials used in the fracturing construction such as fracturing fluid, propping agent and the like do not have the oil displacement function.
Detailed Description
The technical solutions of the present invention will be described in detail below in order to clearly understand the technical features, objects, and advantages of the present invention, but the present invention is not limited to the practical scope of the present invention.
Example 1
The embodiment provides an oil displacement proppant, and a preparation method thereof comprises the following steps:
1500g of fly ash and 1000g of silicon micropowder (the apparent density of the fly ash is 0.35-0.60 g/cm) are added into a mixing granulator at one time3The particle size distribution range is 5-45 μm, and the median particle size D50The heat-resistant temperature of 24 mu m is more than or equal to 500 ℃, and the compressive strength is 83-110 MPa; the apparent density of the silicon micropowder is 2.30-3.90g/cm3Particle size distribution range of 1-6 μm, median particle diameter D504 μm, heat-resisting temperature is more than or equal to 500 ℃,the compressive strength is not lower than that of the fly ash), and stirring is carried out for 1 minute at the speed of 900 revolutions per minute;
42g of 1, 2-di-n-hexyldiselenide were added to the mixing granulator in 10 portions over 5 minutes (during the addition of 1, 2-di-n-hexyldiselenide, the mixing granulator was kept under stirring at 900 rpm), after which stirring was continued at 900 rpm for 1 minute; taking out the materials in the mixing granulator, putting the materials in an oven, and activating and drying the materials for 2 hours at the temperature of 80 ℃;
1500g of the chemically modified mixed powder material is put into a mixing granulator at one time and stirred for 1 minute at the speed of 2000 rpm;
uniformly mixing 40g of acetone and 320g of a prepolymer of thermosetting phenolic resin, and dividing the mixture into two parts, wherein the first part is 324g in weight, and the second part is 36g in weight; the mixture of the prepolymer of the second thermosetting phenolic resin and acetone was stirred uniformly with 6.5g of cetyl alcohol and 8g of an oil-displacing agent (HHSBY-35 from Shandong Baihong New Material Co., Ltd.).
Increasing the stirring speed of a mixing granulator to 3600 revolutions per minute, and adding a first part of mixed solution of the prepolymer of the thermosetting phenolic resin and acetone into the mixing granulator in 10 batches;
increasing the stirring speed of the mixing granulator to 4000 revolutions per minute, and carrying out adhesive granulation for 8 minutes; increasing the stirring speed of the mixing granulator to 5000 r/min, adding the mixed solution of the prepolymer of the second thermosetting phenolic resin and acetone and the mixed solution of hexadecanol and the oil displacement agent into the mixing granulator in 5 batches, and continuously granulating for 2 min to obtain particles with proper size;
and (3) putting the granules obtained by granulation into a drying oven, drying at 90 ℃ for 20 minutes, solidifying at 195 ℃ for 10 minutes, taking out, cooling and sieving to obtain the proppant granules with 20-200 meshes.
The apparent density of the oil displacement proppant provided by the embodiment is 1.07g/cm3The bulk density is 0.47g/cm3。
Example 2
The embodiment provides an oil displacement proppant, and a preparation method thereof comprises the following steps:
once in the mixing granulator1300g of hollow glass microspheres and 1000g of silicon micropowder (the apparent density of the hollow glass microspheres is 0.35-0.60 g/cm)3The particle size distribution range is 5-45 μm, and the median particle size D5024 μm, heat-resisting temperature not less than 500 deg.C, and compressive strength 83-110 MPa; the apparent density of the silicon micropowder is 2.30-3.90g/cm3Particle size distribution range of 1-6 μm, median particle diameter D504 μm, the heat-resistant temperature is more than or equal to 500 ℃, and the compressive strength is not lower than that of the hollow glass microspheres), and stirring is carried out for 1 minute at the speed of 1000 revolutions per minute;
35.8g of 1, 2-di-n-decyldiselenium were added to the mixer-granulator in 10 portions over 5 minutes (the mixer-granulator was kept under stirring at 1000 rpm during the addition of 1, 2-di-n-decyldiselenium), after which stirring was continued at 1000 rpm for 1 minute; taking out the materials in the mixing granulator, putting the materials in an oven, and activating and drying the materials at 90 ℃ for 2 hours;
1350g of the chemically modified mixed powder material is put into a mixing granulator at one time and stirred for 1 minute at the speed of 2000 rpm;
uniformly mixing 35g of ethanol and 280g of prepolymer of thermosetting epoxy resin, and dividing into two parts, wherein the weight of the first part is 280g, and the weight of the second part is 35 g; and uniformly stirring the mixed solution of the prepolymer of the second thermosetting epoxy resin and ethanol, 8g of hexadecanol and 10g of oil displacement agent (DMPS-IB produced by Sichuan Xin Shai Fine chemical Co., Ltd.) for later use.
Increasing the stirring speed of a mixing granulator to 3600 revolutions per minute, and adding a first part of the 280g of the mixed solution of the prepolymer of the thermosetting epoxy resin and the ethanol into the mixing granulator in 10 batches; increasing the stirring speed of the mixing granulator to 4000 revolutions per minute, and carrying out adhesive granulation for 8 minutes; increasing the stirring speed of the mixing granulator to 5000 r/min, adding the mixture of the mixed solution of the 51g of thermosetting phenolic resin prepolymer and acetone and the mixture of cetyl alcohol and an oil displacement agent into the mixture in 5 batches, and continuously granulating for 2 min to obtain particles with proper size;
and (3) putting the granules obtained by granulation into a drying oven, drying at 90 ℃ for 20 minutes, solidifying at 195 ℃ for 10 minutes, taking out, cooling and sieving to obtain the proppant granules with 20-200 meshes.
The apparent density of the oil displacement proppant provided by the embodiment is 1.06g/cm3The bulk density is 0.46g/cm3。
Example 3
The embodiment provides an oil displacement proppant, and a preparation method thereof comprises the following steps:
1700g of hollow glass microspheres and 1100g of bauxite (apparent density of the hollow glass microspheres is 0.35-0.60 g/cm)3The particle size distribution range is 5-45 μm, and the median particle size D5024 μm, heat-resisting temperature not less than 500 deg.C, and compressive strength 83-110 MPa; the bauxite has an apparent density of 2.30-3.90g/cm3Particle size distribution range of 1-6 μm, median particle diameter D504 μm, the heat-resistant temperature is more than or equal to 500 ℃, and the compressive strength is not less than that of the hollow glass microspheres), and stirring is carried out for 1 minute at the speed of 900 revolutions per minute;
47.5g of 1, 2-di-n-hexyldiselenide were added to the mixer-granulator in 10 portions over 5 minutes (during the addition of 1, 2-di-n-hexyldiselenide, the mixer-granulator was kept under stirring at 900 rpm), after which stirring was continued at 900 rpm for 1 minute; taking out the materials in the mixing granulator, putting the materials in an oven, and activating and drying the materials for 2 hours at the temperature of 80 ℃;
1500g of the chemically modified mixed powder material is put into a mixing granulator at one time and stirred for 1 minute at the speed of 1500 revolutions per minute;
after 45g of ethanol and 360g of prepolymer of thermosetting phenolic resin are uniformly mixed, the mixture is divided into two parts, wherein the weight of the first part is 355g, and the weight of the second part is 50 g; uniformly stirring the mixed solution of the prepolymer of the second thermosetting phenolic resin and ethanol with 11g of xylene and 13g of an oil displacement agent (HHSBY-35 produced by Shandong Baihong New Material Co., Ltd.) for later use;
increasing the stirring speed of a mixing granulator to 3600 revolutions per minute, and adding a first part of mixed solution of the prepolymer of the thermosetting phenolic resin and acetone into the mixing granulator in 10 batches;
increasing the stirring speed of the mixing granulator to 4000 revolutions per minute, performing adhesive granulation for 9 minutes, increasing the stirring speed of the mixing granulator to 5000 revolutions per minute, and adding the mixed solution of the prepolymer of the second thermosetting phenolic resin and ethanol, xylene and a compound of an oil displacement agent into the mixture in 5 batches to obtain particles with proper size;
and (3) putting the granules obtained by granulation into a drying oven, drying at 90 ℃ for 20 minutes, solidifying at 190 ℃ for 10 minutes, taking out, cooling and sieving to obtain the proppant granules with 20-200 meshes.
The apparent density of the oil-displacing proppant provided by the embodiment is 1.03g/cm3Bulk density of 0.43g/cm3。
Example 4
The embodiment provides an oil displacement proppant, and a preparation method thereof comprises the following steps:
1500g of hollow glass microspheres and 600g of silicon micropowder (apparent density of hollow glass microspheres is 0.35-0.60 g/cm) are put into a mixing granulator at one time3The particle size distribution range is 5-45 μm, and the median particle size D504 μm, heat-resisting temperature not less than 500 deg.C, and compressive strength 83-110 MPa; the apparent density of the silicon micropowder is 2.30-3.90g/cm3Particle size distribution range of 1-6 μm, median particle diameter D504 μm, the heat-resistant temperature is more than or equal to 500 ℃, and the compressive strength is not lower than that of the hollow glass microspheres), and the mixture is uniformly stirred at the speed of 1200 r/min;
49.3g of 1, 2-di-n-decyldiselenium were added to the mixer-granulator in 10 portions over 5 minutes (during the addition of 1, 2-di-n-decyldiselenium, the mixer-granulator was kept under stirring at 1200 rpm), after which stirring was continued at 1200 rpm for 1 minute; the material in the mixing granulator was taken out and put into an oven, activated and dried at 85 ℃ for 2.5 hours.
1200g of the mixture of the first powder material and the second powder material is put into a mixing granulator at one time, and is stirred for 1 minute at the speed of 1800 rpm;
after 40g of methanol and 300g of prepolymer of thermosetting epoxy resin are uniformly mixed, the mixture is divided into two parts, wherein the weight of the first part is 300g, and the weight of the second part is 40 g; and uniformly stirring the mixed solution of the prepolymer of the second thermosetting epoxy resin and methanol with 9g of hexadecanol and 12g of an oil displacement agent (DMPS-IB produced by Sichuan Xin Shai Fine chemical Co., Ltd.) for later use.
Increasing the stirring speed of a mixing granulator to 4000 rpm, and adding the first part of 300g of the mixed solution of the prepolymer of the thermosetting epoxy resin and methanol into the mixing granulator in 10 batches; the stirring speed of the mixing granulator is increased to 4500 rpm, and the mixture is bonded and granulated for 8 minutes; increasing the stirring speed of the mixing granulator to 5000 r/min, adding the mixture of the mixed solution of the prepolymer of the second thermosetting epoxy resin and methanol and the mixture of hexadecanol and the oil displacement agent into the mixing granulator in 5 batches, and continuously granulating for 2 min to obtain particles with proper size;
and (3) putting the granules obtained by granulation into a drying oven, drying at 90 ℃ for 20 minutes, solidifying at 200 ℃ for 10 minutes, taking out, cooling and sieving to obtain the proppant granules with 20-200 meshes.
The apparent density of the oil-displacing proppant provided by the embodiment is 1.05g/cm3Volume density of 0.45g/cm3。
Comparative example 1
The present comparative example provides a proppant, the method of preparation comprising the steps of:
1500g of hollow glass microspheres and 600g of silicon micropowder (apparent density of hollow glass microspheres is 0.35-0.60 g/cm) are put into a mixing granulator at one time3The particle size distribution range is 5-45 μm, and the median particle size D504 μm, heat-resisting temperature not less than 500 deg.C, and compressive strength 83-110 MPa; the apparent density of the silicon micropowder is 2.30-3.90g/cm3Particle size distribution range of 1-6 μm, median particle diameter D504 μm, the heat-resistant temperature is more than or equal to 500 ℃, and the compressive strength is not lower than that of the hollow glass microspheres), and the mixture is uniformly stirred at the speed of 1200 r/min;
49.3g of 1, 2-di-n-decyldiselenium were added to the mixer-granulator in 10 portions over 5 minutes (during the addition of 1, 2-di-n-decyldiselenium, the mixer-granulator was kept under stirring at 1200 rpm), after which stirring was continued at 1200 rpm for 1 minute; taking out the materials in the mixing granulator, putting the materials in an oven, and activating and drying the materials at 85 ℃ for 2.5 hours to obtain a chemically modified mixed powder material;
1200g of the mixture of the first powder material and the second powder material is put into a mixing granulator at one time, and is stirred for 1 minute at the speed of 1800 rpm;
after 40g of methanol and 300g of prepolymer of thermosetting epoxy resin are uniformly mixed, the mixture is divided into two parts, wherein the weight of the first part is 300g, and the weight of the second part is 40 g;
increasing the stirring speed of a mixing granulator to 4000 rpm, and adding the first part of 300g of the mixed solution of the prepolymer of the thermosetting epoxy resin and methanol into the mixing granulator in 10 batches; the stirring speed of the mixing granulator is increased to 4500 rpm, and the mixture is bonded and granulated for 8 minutes; increasing the stirring speed of the mixing granulator to 5000 r/min, adding the mixed solution of the prepolymer of the second thermosetting epoxy resin and methanol into the mixing granulator in 5 batches, and continuing granulating for 2 min to obtain particles with proper size;
and (3) putting the granules obtained by granulation into a drying oven, drying at 90 ℃ for 20 minutes, solidifying at 200 ℃ for 10 minutes, taking out, cooling and sieving to obtain the proppant granules with 20-200 meshes.
The apparent density of the oil displacement proppant provided by the comparative example is 1.05g/cm3Volume density of 0.45g/cm3。
Comparative example 2
The present comparative example provides a proppant, the method of preparation comprising the steps of:
1500g of hollow glass microspheres and 600g of silicon micropowder (apparent density of hollow glass microspheres is 0.35-0.60 g/cm) are put into a mixing granulator at one time3The particle size distribution range is 5-45 μm, and the median particle size D504 μm, heat-resisting temperature not less than 500 deg.C, and compressive strength 83-110 MPa; the apparent density of the silicon micropowder is 2.30-3.90g/cm3Particle size distribution range of 1-6 μm, median particle diameter D504 μm, the heat-resistant temperature is more than or equal to 500 ℃, and the compressive strength is not lower than that of the hollow glass microspheres), and the mixture is uniformly stirred at the speed of 1200 r/min;
138g of an aqueous potassium hydroxide solution having a concentration of 12.5% by mass were added to the mixing granulator in 10 portions over a period of 5 minutes (during the addition of the aqueous potassium hydroxide solution, the mixing granulator was kept under stirring at 1200 rpm), after which stirring was continued at 1200 rpm for 2 minutes, and subsequently 64g of an aqueous glutaraldehyde solution having a concentration of 50% by mass were added to the granulator in 5 portions over a period of 2.5 minutes (during the addition of the aqueous glutaraldehyde solution, the mixing granulator was kept under stirring at 1200 rpm), after which stirring was continued at 1200 rpm for 1 minute; and taking the materials in the mixing granulator out, putting the materials in an oven, and activating and drying the materials at 85 ℃ for 2.5 hours to obtain the chemically modified mixed powder material.
1200g of the mixture of the first powder material and the second powder material is put into a mixing granulator at one time, and is stirred for 1 minute at the speed of 1800 rpm;
after 40g of methanol and 300g of prepolymer of thermosetting epoxy resin are uniformly mixed, the mixture is divided into two parts, wherein the weight of the first part is 300g, and the weight of the second part is 40 g; and uniformly stirring the mixed solution of the prepolymer of the second thermosetting epoxy resin and methanol with 9g of hexadecanol and 12g of an oil displacement agent (DMPS-IB produced by Sichuan Xin Shai Fine chemical Co., Ltd.) for later use.
Increasing the stirring speed of a mixing granulator to 4000 rpm, and adding the first part of 300g of the mixed solution of the prepolymer of the thermosetting epoxy resin and methanol into the mixing granulator in 10 batches; the stirring speed of the mixing granulator is increased to 4500 rpm, and the mixture is bonded and granulated for 8 minutes; increasing the stirring speed of the mixing granulator to 5000 r/min, adding the mixture of the mixed solution of the prepolymer of the second thermosetting epoxy resin and methanol and the mixture of hexadecanol and the oil displacement agent into the mixing granulator in 5 batches, and continuously granulating for 2 min to obtain particles with proper size;
and (3) putting the granules obtained by granulation into a drying oven, drying at 90 ℃ for 20 minutes, solidifying at 200 ℃ for 10 minutes, taking out, cooling and sieving to obtain the proppant granules with 20-200 meshes.
The apparent density of the oil displacement proppant provided by the comparative example is 1.75g/cm3Volume density of 0.95g/cm3。
Comparative example 3
The comparative example provides a hollow glass microsphere modified by potassium hydroxide and glutaraldehyde, and the preparation method comprises the following steps:
2100g of hollow glass microspheres (apparent density of the hollow glass microspheres is 0.35-0.60 g/cm) were put into a mixing granulator at one time3The particle size distribution range is 5-45 μm, and the median particle size D504 μm, the heat-resisting temperature is more than or equal to 500 ℃, and the compressive strength is 83-110MPa), and the mixture is uniformly stirred at the speed of 1200 r/min;
138g of an aqueous potassium hydroxide solution having a concentration of 12.5% by mass were added to the mixing granulator in 10 portions over a period of 5 minutes (during the addition of the aqueous potassium hydroxide solution, the mixing granulator was kept under stirring at 1200 rpm), after which stirring was continued at 1200 rpm for 2 minutes, and subsequently 64g of an aqueous glutaraldehyde solution having a concentration of 50% by mass were added to the granulator in 5 portions over a period of 2.5 minutes (during the addition of the aqueous glutaraldehyde solution, the mixing granulator was kept under stirring at 1200 rpm), after which stirring was continued at 1200 rpm for 1 minute; and taking out the materials in the mixing granulator, putting the materials in an oven, and activating and drying the materials at 85 ℃ for 2.5 hours to obtain the chemically modified hollow glass microspheres.
When the modified hollow glass microspheres are observed under a microscope of 40 times, about 50% of the hollow glass microspheres are broken.
The comparative example also provides a hollow glass microsphere modified by 1, 2-di-n-decyl diselenide, and the preparation method comprises the following steps:
2100g of hollow glass microspheres (apparent density of the hollow glass microspheres is 0.35-0.60 g/cm) were put into a mixing granulator at one time3The particle size distribution range is 5-45 μm, and the median particle size D504 μm, the heat-resisting temperature is more than or equal to 500 ℃, and the compressive strength is 83-110MPa), and the mixture is uniformly stirred at the speed of 1200 r/min;
49.3g of 1, 2-di-n-decyldiselenium were added to the mixer-granulator in 10 portions over 5 minutes (during the addition of 1, 2-di-n-decyldiselenium, the mixer-granulator was kept under stirring at 1200 rpm), after which stirring was continued at 1200 rpm for 1 minute; the material in the mixing granulator was taken out and put into an oven, activated and dried at 85 ℃ for 2.5 hours.
Observing the modified hollow glass microsphere under a 40-fold microscope, wherein the crushing proportion of the hollow glass microsphere is less than 5 percent and is far lower than the crushing proportion of the hollow glass microsphere modified by potassium hydroxide and glutaraldehyde provided by the comparative example in the modification process.
Therefore, the strength of the hollow glass microspheres is reduced by modifying the hollow glass microspheres by potassium hydroxide and glutaraldehyde, and if the hollow glass microspheres modified by the potassium hydroxide and the glutaraldehyde are used as the raw materials of the proppant, the compressive property of the proppant is not facilitated. In addition, if the hollow glass microspheres modified by potassium hydroxide and glutaraldehyde are used as the raw material of the proppant, the density of the proppant is increased due to the breakage of the hollow glass microspheres, which is one of the reasons that the density of the proppant in comparative example 2 is much higher than that of the proppant provided in examples 1 to 4.
Comparative example 4
The present comparative example provides a proppant, the method of preparation comprising the steps of:
1500g of hollow glass microspheres and 600g of silicon micropowder (apparent density of hollow glass microspheres is 0.35-0.60 g/cm) are put into a mixing granulator at one time3The particle size distribution range is 5-45 μm, and the median particle size D504 μm, heat-resisting temperature not less than 500 deg.C, and compressive strength 83-110 MPa; the apparent density of the silicon micropowder is 2.30-3.90g/cm3Particle size distribution range of 1-6 μm, median particle diameter D504 μm, the heat-resistant temperature is more than or equal to 500 ℃, and the compressive strength is not lower than that of the hollow glass microspheres), and the mixture is uniformly stirred at the speed of 1200 r/min;
49.3g of 1, 2-di-n-decyldiselenium were added to the mixer-granulator in 10 portions over 5 minutes (during the addition of 1, 2-di-n-decyldiselenium, the mixer-granulator was kept under stirring at 1200 rpm), after which stirring was continued at 1200 rpm for 1 minute; and taking the materials in the mixing granulator out, putting the materials in an oven, and activating and drying the materials at 85 ℃ for 2.5 hours to obtain the chemically modified mixed powder material.
1200g of the mixture of the first powder material and the second powder material is put into a mixing granulator at one time, and is stirred for 1 minute at the speed of 1800 rpm;
40g of methanol and 300g of a prepolymer of the thermosetting epoxy resin are mixed uniformly, and then the mixture is stirred uniformly with 9g of hexadecanol and 12g of an oil displacement agent (DMPS-IB produced by Sichuan Xin Shai Fine chemical Co., Ltd.) for later use.
The stirring speed of the mixing granulator is increased to 4000 revolutions per minute, and the mixed solution of the prepolymer of the thermosetting epoxy resin, methanol, hexadecanol and an oil displacement agent (DMPS-IB produced by Sichuan Xinrui chemical Co., Ltd.) is added into the mixing granulator in 10 batches; the stirring speed of the mixing granulator is increased to 4500 rpm, and the mixture is bonded and granulated for 8 minutes; increasing the stirring speed of the mixing granulator to 5000 r/min, and continuing granulating for 2 min to obtain particles with proper size;
and (3) putting the granules obtained by granulation into a drying oven, drying at 90 ℃ for 20 minutes, solidifying at 200 ℃ for 10 minutes, taking out, cooling and sieving to obtain the proppant granules with 20-200 meshes.
The proppant provided in this comparative example had an apparent density of 1.05g/cm3Volume density of 0.45g/cm3。
TABLE 1
The flooding proppant provided in examples 1-4 and the proppant products provided in comparative examples 1-2 and 4 were subjected to performance tests, and the test results are shown in table 1.
The test of roundness/sphericity and breakage rate is referred to the fracturing propping agent and performance index and test recommendation method in accordance with the oil and gas industry standard SY/T5108-2006 of the people's republic of China.
Effective displacement of reservoir oil volume ratio Vwater/VproppantThe determination is determined by referring to a short-term conductivity evaluation recommendation method of a SYT6302-2009 fracturing proppant pack and an indoor evaluation method of a surfactant applied to an SYT5753-1995 oilfield stimulation well injection measure. It should be noted that the conductivity of the flooding proppant was not measured. Measurement of Vwater/VproppantBriefly described, a volume V is definedproppantThe flooding proppant provided in examples 1 to 4 was placed in a diversion chamber with an effective closure stress of 30MPa, distilled water as the inlet fluid of the diversion chamber at a flow rate of 3mL/min, and every 50V were collected in sequenceproppantThe outlet fluid of the diversion chamber is numbered as 1,2, 3, 4, … … and m (m is a positive integer), the outlet fluid is subjected to interfacial tension measurement, the collection is stopped when the interfacial tension of the outlet fluid of the diversion chamber is more than or equal to 0.1mN/m, the number of the fluid sample is recorded as n (n is a positive integer, n is less than or equal to m), and then V is obtainedwater/Vproppant50 × (n-1). The interfacial tension is measured according to a rotating drop method specified in oil and gas industry standard SY/T5370-2018 surface and interfacial tension measuring method of the people's republic of China, the measuring temperature is 25 +/-0.2 ℃, and an adopted instrument is an interfacial tension tester Texas-500C produced by the United states Keno industry Co.
From the results in table 1, it can be seen that the apparent density, the bulk density, the sphericity/sphericity and the pressure resistance of the oil-displacing proppant provided in examples 1 to 4 are all similar, the effective oil-displacing volume ratio (volume of produced water of the oil-displacing agent/volume of the oil-displacing proppant, Vwater/vpropant) of the oil-displacing proppant is not less than 1000, and the interfacial tension of produced water of the oil-displacing agent is less than 0.1mN/m, but the proppant provided in comparative example 1 has no oil-displacing effect basically.
The proppant provided in comparative example 1 has no porogen added, and the apparent density and bulk density are the same as those of the proppant provided in example 4, which indicates that the addition or absence of the porogen is not a critical factor for determining the density of the proppant.
As can be seen from table 1 and comparative example 3, the proppant provided in comparative example 2 has a structure damaged due to modification of the hollow glass microspheres with potassium hydroxide and glutaraldehyde water during the preparation process, resulting in much higher fracture rate and packing layer deformation amount of the proppant provided in comparative example 2 than the proppant provided in examples 1 to 4 modified with diselenide compound.
As can be seen from table 1, in the proppant provided in comparative example 4, the second mixture of the thermosetting resin binder and the organic solvent, the oil-displacing agent, and the pore-forming agent is not added in the later stage of the adhesive granulation process, but the oil-displacing agent, the pore-forming agent, and the mixture of all the thermosetting resin binder and the organic solvent are added into the chemically modified mixed powder material for adhesive granulation. Although the obtained proppant has good oil displacement effect, density, roundness/sphericity and other performances, the fracture rate and the deformation amount of a filling layer are obviously higher than those of the oil displacement proppant provided in examples 1-4, because the proppant provided in comparative example 4 has a certain number of micropores in the interior except the surface, and cannot provide effective compressive strength when a fracture rate test is carried out.
In addition, the proppants provided in examples 1-4 were placed in an oven at 160 ℃ and heated for 30 days, and then the fracture rate and V were again performedwater/VproppantThe results of the tests are shown in Table 2. The results in Table 2 show that the proppants provided in examples 1-4 still maintain good performance specifications after long-term high temperature failure.
TABLE 2
The oil-displacing proppant provided by the invention can keep basic suspension in clear water or slickwater, so that the proppant can be carried and laid by using the clear water or slickwater, has larger laying height and length in cracks, and can play an oil-displacing function in a larger range. The oil-displacing proppant provided by the invention has a long-term working temperature of more than or equal to 160 ℃, can meet the requirements of fracturing clear water or slickwater fracturing construction of deep high-temperature oil and gas wells, has low breaking rate under the closed pressure of 10-60MPa, is beneficial to keeping higher flow conductivity of a proppant filling layer, and can meet the dual requirements of fracture support and oil displacement.
Claims (26)
1. An oil displacement proppant, the apparent density of the oil displacement proppant is 1.00-1.08g/cm3The bulk density is 0.40-0.50g/cm3The raw materials of the oil displacement proppant comprise a prepolymer of a thermosetting resin adhesive, an organic solvent, a chemically modified mixed powder material, a pore-forming agent and an oil displacement agent; wherein the content of the first and second substances,
the chemically modified mixed powder material comprises a chemically modified first powder material and a chemically modified second powder material;
the oil displacement proppant comprises, by taking the total weight of raw materials of the oil displacement proppant as 100%, 40-55% of the chemically modified first powder material, 20-33% of the chemically modified second powder material, 15-20% of a prepolymer of a thermosetting resin adhesive, 2-4% of an organic solvent, 0.1-2% of a pore-forming agent and 0.1-2% of an oil displacement agent;
wherein the chemically modified first powder material comprises chemically modified fly ash and/or chemically modified hollow glass microspheres; the chemically modified second powder material comprises chemically modified silicon micropowder and/or chemically modified bauxite; when the first powder material and the second powder material are chemically modified, the used modifier comprises 1, 2-di-n-hexyl diselenide and/or 1, 2-di-n-decyl diselenide;
wherein the oil displacement agent meets the following conditions: after the crude oil/formation water interfacial tension is endured for 24 hours at the temperature of more than 200 ℃, the crude oil/formation water interfacial tension can still be reduced to less than 0.1 mN/m.
2. The flooding proppant of claim 1, wherein,
the apparent density of the first powder material before chemical modification is 0.35-0.70g/cm3The particle size distribution range before chemical modification is 5-45 μm;
the apparent density of the second powder material before chemical modification is 2.30-3.90g/cm3The particle size distribution range before chemical modification is 1-6 μm.
3. The flooding proppant of claim 2, wherein the first powder material has a median particle size, D, prior to chemical modification50And 24 μm.
4. The flooding proppant of claim 2, wherein the second powder material has a median value prior to chemical modificationParticle diameter D50And was 4 μm.
5. The flooding proppant of any one of claims 1-4, wherein,
when the first powder material and the second powder material are chemically modified, the weight ratio of the modifier to the chemically modified mixed powder material is 1:200-1: 20.
6. The flooding proppant of claim 1, wherein the prepolymer of the thermosetting resin binder is in a liquid state having a viscosity of 500-6000 mPa-s at 25 ℃.
7. The flooding proppant of claim 6, wherein the prepolymer of the thermosetting resin binder comprises one or a combination of two or more of a prepolymer of a thermosetting epoxy resin, a prepolymer of a thermosetting phenolic resin, and a prepolymer of a thermosetting polyurethane resin.
8. The flooding proppant of claim 1, wherein the pore-forming agent comprises one or a combination of two or more of dipropyl phthalate, cetyl alcohol, and xylene.
9. The flooding proppant of claim 1, wherein,
the heat-resistant temperature of the first powder material before chemical modification is more than or equal to 500 ℃, and the compressive strength of the first powder material before chemical modification is 83-110 MPa;
the heat-resistant temperature of the second powder material before chemical modification is more than or equal to 500 ℃, and the compressive strength of the second powder material before chemical modification is not lower than that of the first powder material before chemical modification.
10. The flooding proppant of claim 1, wherein the organic solvent comprises one or a combination of two or more of methanol, ethanol, and acetone.
11. The flooding proppant of claim 1, wherein the flooding proppant has a particle size of 20-200 mesh.
12. The flooding proppant of claim 11, wherein the proppant has a particle size of 20-40 mesh, 40-70 mesh, 70-100 mesh, or 100-200 mesh.
13. The method of making an flooding proppant of any one of claims 1-12, comprising the steps of:
adding a first part of mixture of thermosetting resin adhesive and organic solvent into the chemically modified mixed powder material, and performing adhesion granulation;
adding a mixture obtained by mixing a second mixture of thermosetting resin adhesive and organic solvent with an oil displacement agent and a pore-forming agent at the later stage of the bonding and granulating process to obtain particles;
drying, solidifying, cooling and sieving the particles to obtain the oil displacement proppant;
wherein the weight ratio of the mixture of the first part of thermosetting resin adhesive and organic solvent to the mixture of the second part of thermosetting resin adhesive and organic solvent is 97:3-85: 15; the sum of the mass of the mixture of the first part of thermosetting resin binder and the organic solvent and the mass of the mixture of the second part of thermosetting resin binder and the organic solvent is the sum of the mass of the thermosetting resin binder and the organic solvent in the raw oil-displacing proppant component; wherein the sum of the mass of the thermosetting resin binder in the mixture of the first part of thermosetting resin binder and the organic solvent and the mass of the thermosetting resin binder in the mixture of the second part of thermosetting resin binder and the organic solvent is the total mass of the thermosetting resin binders in the oil-displacing proppant raw material component, and the sum of the mass of the organic solvent in the mixture of the first part of thermosetting resin binder and the organic solvent and the mass of the organic solvent in the mixture of the second part of thermosetting resin binder and the organic solvent is the total mass of the organic solvent in the oil-displacing proppant raw material component.
14. The preparation method according to claim 13, wherein the chemically modified mixed powder material is prepared by a modification method comprising the steps of:
uniformly mixing the first powder material and the second powder material to obtain a mixed powder material;
and adding a modifier into the mixed powder material, and then activating at a preset temperature and a preset time to obtain the chemically modified mixed powder material.
15. The method of claim 14, wherein the predetermined temperature is 60-120 ℃.
16. The method of claim 15, wherein the predetermined temperature is 60-100 ℃.
17. The method of claim 16, wherein the predetermined temperature is 70-90 ℃.
18. The production method according to claim 14, wherein the predetermined time is 1 to 6 hours.
19. The production method according to claim 18, wherein the predetermined time is 1 to 4 hours.
20. The production method according to claim 19, wherein the predetermined time is 2 to 3 hours.
21. The method according to claim 13, wherein the drying is carried out at a temperature of 60 to 100 ℃ for 10 to 30 minutes.
22. The method according to claim 21, wherein the drying is carried out at a temperature of 80 to 100 ℃ for 20 to 30 minutes.
23. The method as claimed in claim 13, wherein the curing temperature is 150 ℃ to 200 ℃ and the curing time is 5 to 30 minutes.
24. The method as claimed in claim 23, wherein the curing temperature is 180-200 ℃ and the curing time is 5-15 minutes.
25. The method of claim 13, wherein the total time for the adhesive granulation is 5 to 15 minutes.
26. The preparation method according to claim 25, wherein the total time of the adhesive granulation is 8 to 12 minutes, wherein the adhesive granulation time is 6 to 10 minutes before adding the mixture obtained by mixing the second mixture of the thermosetting resin binder and the organic solvent with the oil displacing agent and the pore-forming agent, and the adhesive granulation time is 2 to 3 minutes after adding the mixture obtained by mixing the second mixture of the thermosetting resin binder and the organic solvent with the oil displacing agent and the pore-forming agent.
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