CN115232608A - High-temperature-resistant consolidated precoated sand and preparation method thereof - Google Patents
High-temperature-resistant consolidated precoated sand and preparation method thereof Download PDFInfo
- Publication number
- CN115232608A CN115232608A CN202210613790.5A CN202210613790A CN115232608A CN 115232608 A CN115232608 A CN 115232608A CN 202210613790 A CN202210613790 A CN 202210613790A CN 115232608 A CN115232608 A CN 115232608A
- Authority
- CN
- China
- Prior art keywords
- sand
- epoxy resin
- temperature
- thermosetting epoxy
- coated
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Classifications
-
- 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
- C09K8/50—Compositions for plastering borehole walls, i.e. compositions for temporary consolidation of borehole walls
- C09K8/504—Compositions based on water or polar solvents
- C09K8/506—Compositions based on water or polar solvents containing organic compounds
- C09K8/508—Compositions based on water or polar solvents containing organic compounds macromolecular compounds
- C09K8/5083—Compositions based on water or polar solvents containing organic compounds macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
-
- 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
- C09K8/50—Compositions for plastering borehole walls, i.e. compositions for temporary consolidation of borehole walls
-
- 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
- C09K8/50—Compositions for plastering borehole walls, i.e. compositions for temporary consolidation of borehole walls
- C09K8/504—Compositions based on water or polar solvents
- C09K8/506—Compositions based on water or polar solvents containing organic compounds
- C09K8/508—Compositions based on water or polar solvents containing organic compounds macromolecular compounds
- C09K8/5086—Compositions based on water or polar solvents containing organic compounds macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
-
- 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
- C09K8/56—Compositions for consolidating loose sand or the like around wells without excessively decreasing the permeability thereof
-
- 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
- C09K8/56—Compositions for consolidating loose sand or the like around wells without excessively decreasing the permeability thereof
- C09K8/57—Compositions based on water or polar solvents
- C09K8/575—Compositions based on water or polar solvents containing organic compounds
- C09K8/5751—Macromolecular compounds
- C09K8/5753—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
-
- 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
- C09K8/56—Compositions for consolidating loose sand or the like around wells without excessively decreasing the permeability thereof
- C09K8/57—Compositions based on water or polar solvents
- C09K8/575—Compositions based on water or polar solvents containing organic compounds
- C09K8/5751—Macromolecular compounds
- C09K8/5755—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
Abstract
The invention provides high-temperature-resistant consolidated precoated sand and a preparation method thereof, belonging to the technical field of chemical profile control and sand prevention. The high-temperature-resistant consolidated precoated sand comprises skeleton sand, a thermosetting epoxy resin layer coated on the surface of the skeleton sand and a hydrophobic polymer layer coated on the thermosetting epoxy resin layer; the hydrophobic polymer in the hydrophobic polymer layer is obtained by polymerizing 2-acrylamide-2-methylpropanesulfonic acid and acrylamide. The thermosetting epoxy resin layer is adopted to coat the skeleton sand, so that the skeleton layer and the water-blocking and oil-permeable functional layer are connected; 2-acrylamide-2-methylpropanesulfonic acid and acrylamide are copolymerized to obtain a hydrophobic polymer, so that the coated sand has good oil permeability and water resistance. The high-temperature-resistant consolidated precoated sand disclosed by the invention has extremely strong hydrophobic property and high-temperature stability, is applied to the high-temperature environment of a high-temperature huff and puff heavy oil well, and has a better water control profile control or sand prevention effect.
Description
Technical Field
The invention belongs to the technical field of chemical profile control and sand prevention, and particularly relates to high-temperature-resistant consolidated coated sand and a preparation method thereof.
Background
The heavy oil reservoir of the oil field in the western Henan region has the characteristics of shallow burial, thin thickness, high crude oil viscosity, low diagenesis degree and loose reservoir cementation. The heavy oil reservoir is mainly produced in a steam huff and puff mode, the temperature is generally above 350 ℃, and the stratum structure is damaged under the action of high-temperature steam to erode asphalt and minerals and repeatedly stimulate the reservoir, so that the sand production of the stratum is serious, and even the stratum is empty. As the formation sand production progresses, steam channeling channels can be formed among oil wells, and the steam heat utilization rate and the oil well yield are seriously influenced. And high-speed fluid generated by steam channeling further aggravates the problem of sand production, so that inter-well and unidirectional steam channeling gradually change into bidirectional steam channeling, multi-well mutual channeling or sheet steam channeling, and the problems of side water and bottom water bulge and the like are caused, so that the water content of produced liquid of an oil well is increased, and the crude oil production degree is influenced.
At present, aiming at the problem of sand production of a heavy oil reservoir oil well, in the prior art, chemical sand control methods such as a high-temperature sand consolidation agent and the like are mainly adopted to consolidate loose stratum sand particles to form a sand blocking barrier with certain strength and permeability, so that the aims of oil production and sand control are fulfilled. But due to the heterogeneity of the formation permeability, the chemical sand control consolidation strength is unstable, the effective period is short, and the cost is high. Moreover, the precoated sand in the prior art has poor heat resistance, and has low consolidation strength in a high-temperature environment of steam huff and puff of a heavy oil reservoir, so that the basic water-blocking sand-prevention requirement is difficult to meet; most of the high-temperature resistant precoated sand has no oil-permeable and water-resistant functions, and is difficult to meet the requirements of water control and sand prevention.
Disclosure of Invention
One of the purposes of the invention is to provide high-temperature-resistant consolidated precoated sand which has both oil-permeable and water-resistant functions and high-temperature resistance.
The invention also aims to provide a preparation method of the high-temperature-resistant consolidated precoated sand, which is beneficial to obtaining the precoated sand with excellent high-temperature resistance, oil permeability and water resistance.
The invention relates to high-temperature-resistant consolidated precoated sand, which adopts the technical scheme that:
the high-temperature-resistant curable precoated sand comprises skeleton sand, a thermosetting epoxy resin layer coated on the surface of the skeleton sand and a hydrophobic polymer layer coated on the thermosetting epoxy resin layer; the hydrophobic polymer in the hydrophobic polymer layer is obtained by polymerizing 2-acrylamide-2-methylpropanesulfonic acid and acrylamide.
The high-temperature-resistant consolidated precoated sand disclosed by the invention adopts the thermosetting epoxy resin layer to coat the skeleton sand, the ether bond inherent in the epoxy resin molecular chain can provide certain hydrophobicity, and the polar hydroxyl can show high adhesion to the skeleton sand, so that the thermosetting epoxy resin layer plays a role in connecting the skeleton layer and the water-blocking and oil-permeable functional layer; the thermosetting epoxy resin is convenient to cure, can be cured within the range of 0-180 ℃, forms a stable net structure after reacting and curing with a curing agent, has high compressive strength which can reach over 9MPa, has good high temperature resistance, and can still keep the compressive strength between 2.75-4.30 MPa after being burned at the high temperature of 350 ℃ for 2 hours.
The hydrophobic polymer obtained by copolymerizing 2-acrylamide-2-methylpropanesulfonic acid and acrylamide has stronger stability at high temperature, has strong hydrophobic amino groups, shows a lotus effect, enables the hydrophobic polymer layer to play roles of enhancing hydrophobic property, providing selective passing capacity of oil and water and the like, and is used as a water-blocking and oil-permeable functional layer to endow the high-temperature-resistant consolidated precoated sand with good oil-permeable and water-permeable properties.
Through the matching of the thermosetting epoxy resin layer and the hydrophobic polymer layer, the high-temperature-resistant consolidated coated sand disclosed by the invention has extremely strong hydrophobic property and high-temperature stability, and has a better water-controlling profile-controlling or sand-preventing effect when being applied to a high-temperature environment of a high-temperature huff and puff heavy oil well.
Preferably, the epoxy value of the thermosetting epoxy resin is 0.41 to 0.47. The thermosetting epoxy resin in the thermosetting epoxy resin layer is bisphenol A diglycidyl ether, namely E44 bisphenol A epoxy resin. The bisphenol A diglycidyl ether is convenient to cure, can bond the skeleton sand and the water-blocking and oil-permeable functional layer together under acidic or alkaline conditions, and has higher compressive strength and better high-temperature resistance after being cured.
According to the invention, epoxy resins are classified according to epoxy values, for example, E44 epoxy resin represents that the average epoxy value is 44/100, and the epoxy value N/100 is 0.41-0.47; e51 epoxy resin, which represents that the average epoxy value is 51/100, and the epoxy value N/100 is 0.48-0.54.
Preferably, the particle size of the skeleton sand is 40-120 meshes. The skeleton sand with the particle size can ensure that a solidified body has excellent permeability. The particle sizes of A-B mesh and A/B mesh in the invention mean the passing rate of the particles on the mesh screen of A mesh and the passing rate on the mesh screen of B mesh are 98%.
Preferably, in order to further improve the permeability of the consolidated precoated sand, the particle size of the skeleton sand is 20/40 meshes or 40/70 meshes.
Preferably, the skeleton sand is quartz sand. The quartz sand has low cost, high strength and high temperature resistance, a large number of OH groups are also arranged on the surface of the quartz sand, the quartz sand can be combined with resin, the film covering strength is improved, the strength after film covering can be 3-4 times higher than that of the quartz sand, the components of the quartz sand are close to formation sand, the affinity with the formation is good, the application in formation sand control is facilitated, and the damage and the pollution to the formation are not easily caused.
Preferably, the sphericity of the quartz sand is greater than 0.6. The quartz sand has small specific surface area, can obtain the coated sand with the same strength, consumes less resin during coating, and has low cost investment. And the precoated sand made of the quartz sand with good sphericity has smaller accumulation volume, is used for sand prevention and has better effect.
Further, the quartz sand is selected from quartz sand with a clean and smooth surface.
Preferably, the mass ratio of the 2-acrylamido-2-methylpropanesulfonic acid to the acrylamide is (5-8) to (10-15). The 2-acrylamide-2-methylpropanesulfonic acid and acrylamide in the mass ratio are copolymerized, and the obtained hydrophobic polymer has excellent hydrophobic effect and high-temperature stability.
The preparation method of the high-temperature-resistant consolidated precoated sand adopts the technical scheme that:
a preparation method of the high-temperature-resistant consolidated precoated sand comprises the following steps:
1) Mixing the skeleton sand with thermosetting epoxy resin to coat the thermosetting epoxy resin on the surface of the skeleton sand, and then stirring and mixing the skeleton sand with a dispersing agent to obtain resin coated sand; the dispersing agent is calcium carbonate powder;
2) Carrying out acid washing on the resin coated sand to remove a dispersing agent, so as to obtain coated particles;
3) And (3) soaking the coated particles in a hydrophobic polymer solution, and drying to obtain the coating.
According to the invention, calcium carbonate powder is used as a dispersing agent, so that the effects of caking resistance and adhesion resistance can be exerted, and the resin coated sand is prevented from agglomerating; after the film-coated resin is solidified and cooled, the calcium carbonate powder is removed by acid washing, so that the exposed surface area of the resin can be increased, the solidifying contact area of the thermosetting epoxy resin is increased, and the improvement of the compressive strength after solidification is facilitated; in addition, a small amount of calcium carbonate powder remains in the thermosetting epoxy resin, which can also increase the hardness of the precoated sand. Therefore, the preparation method can obtain the precoated sand with higher compressive strength and hardness after consolidation, and is beneficial to the application in sand control of a heavy oil well.
Preferably, in order to rapidly and thoroughly clean calcium carbonate on the surface of the resin-coated sand, expose the surface of the thermosetting epoxy resin and enlarge the consolidation contact surface, the acid cleaning is to soak the resin-coated sand for 3 to 4 hours by using dilute hydrochloric acid.
Further, the mass concentration of the dilute hydrochloric acid is 3-4%. For example, the dilute hydrochloric acid has a mass concentration of 3%.
Preferably, in the step 3), the drying temperature is 50-60 ℃ and the drying time is 8-12 hours. The drying can be carried out in an oven, and the temperature of the oven is controlled to be 50-60 ℃ in the drying process. After drying treatment, the hydrophobic polymer can be solidified on the surface of the coated particle to form a hydrophobic polymer layer.
Preferably, the mass of the thermosetting epoxy resin in the thermosetting epoxy resin layer is 5.5-6.5% of the mass of the skeleton sand. The mass ratio is favorable for fully coating the thermosetting epoxy resin on the surface of the skeleton sand, is not easy to agglomerate, is favorable for bonding the skeleton sand and the hydrophobic polymer layer, and can ensure the excellent curing strength of the high-temperature-resistant curable precoated sand.
Preferably, the mass of the calcium carbonate powder is 2.0-3.0% of the mass of the thermosetting epoxy resin. The calcium carbonate powder with the mass ratio can fully play the roles of anti-caking and anti-adhesion, the calcium carbonate powder on the surface can be conveniently removed, and the residual part of the calcium carbonate powder in the coating can further improve the strength of the coated particles.
Preferably, the calcium carbonate powder has a particle size of the order of nanometers, i.e., a particle size of 1 to 100nm.
Preferably, the hydrophobic polymer solution is obtained by diluting a hydrophobic polymer by 4-6 times with acetone; in the step 3), the mass ratio of the coated particles to the hydrophobic polymer solution is 1:2, the soaking time is 4-6 h.
Preferably, in the step 3), the soaking is performed at normal temperature and normal pressure. In order to bond the hydrophobic polymer on the surface of the thermosetting epoxy resin layer, the solution of the hydrophobic polymer after the coating particles are immersed is stirred in the soaking process of the step 3), and the stirring time is preferably 4-6 h.
Preferably, in the step 3), the hydrophobic polymer is obtained by polymerizing 2-acrylamido-2-methylpropanesulfonic acid and acrylamide, and the mass ratio of the 2-acrylamido-2-methylpropanesulfonic acid to the acrylamide is (5-8) to (10-15). The hydrophobic polymer with the mass ratio is beneficial to the passing of small molecules of a curing agent and the curing of thermosetting epoxy resin while forming a hydrophobic polymer layer to improve the hydrophobic performance.
Preferably, in step 3), the hydrophobic polymer is prepared by a method comprising the following steps: adjusting the pH value of a mixed aqueous solution of 2-acrylamide-2-methylpropanesulfonic acid and acrylamide to 6-8, adding an initiator, and carrying out polymerization reaction for 6 hours at the temperature of 70-80 ℃ to obtain the product; the mass concentration of the 2-acrylamide-2-methylpropanesulfonic acid in the mixed aqueous solution is 5-8%, and the mass concentration of the acrylamide is 10-15%.
Preferably, the initiator is ammonium persulfate, and the concentration of the ammonium persulfate is 0.05-0.1% of the mass of the mixed water solution.
Preferably, the polymerization is carried out at 75 ℃ for 6h.
Preferably, the dilution factor is 4 to 8; the diluting agent adopted in the dilution is an organic solvent, such as acetone, a viscous liquid hydrophobic polymer is obtained through reaction, the hydrophobic polymer is insoluble in water, and the liquid viscosity can be reduced through the dispersion of the organic solvent in the dilution step.
Preferably, in order to ensure that the film-coated particles can be immersed in the hydrophobic polymer solution, the volume ratio of the hydrophobic polymer solution to the quartz sand is 2.
Preferably, the skeleton sand and the thermosetting epoxy resin in the step 1) are mixed, stirred and mixed at 80-85 ℃ for 30-40 min. The temperature range has the beneficial effects that the epoxy resin E-44 can bear the high temperature of 100 ℃ at most, the activity of an epoxy group is kept within 100 ℃, the consistency of the resin can be reduced, and the uniform film coating is facilitated.
Preferably, the stirring and mixing process further comprises a cooling step, wherein the cooling step is to cool the mixture to below 25 ℃ so that the calcium carbonate powder is compounded on the thermosetting epoxy resin to form the resin-coated sand.
Preferably, before the framework sand and the thermosetting epoxy resin are mixed, the framework sand is sequentially subjected to purification treatment and surface degreasing treatment. The cleaning process may remove grease and debris, such as crude oil and clay, from the surface of the skeletal sand. The substances such as grease, clay and the like can be removed, so that the influence of the substances such as grease, clay and the like on the quality of the epoxy resin coating can be avoided, and the coating of the coating support shell can be avoided.
Further, the purification treatment adopts the methods of rubbing, washing or flotation and the like, and then drying treatment is carried out, and the mud content of the skeleton sand is controlled to be less than 0.5%, the micro powder content is controlled to be less than 1%, and the water content is controlled to be less than 0.2%.
Preferably, the degreasing treatment is to treat the skeleton sand at a constant temperature of 350-400 ℃ for 2h, and the temperature range can burn off grease and decompose and gasify the grease, so that the high-temperature resistance of the precoated sand is improved.
Preferably, the high-temperature-resistant consolidated coated sand is applied to sand control or water control profile control of a heavy oil well. The high-temperature-resistant consolidated precoated sand has excellent water-blocking and oil-penetrating properties, is beneficial to water-blocking sand prevention or water-controlling profile control in a heavy oil well, has good high-temperature resistance, and can stably play a role in huff and puff thermal recovery of the heavy oil well.
Preferably, when the high-temperature-resistant consolidated coated sand is applied to sand control or water control profile control of a thick oil well, the method comprises the following steps: injecting the high temperature resistant consolidated coated sand into a formation. When the high-temperature-resistant consolidated precoated sand is applied, the sand-carrying fluid is fed into a stratum, a water-blocking sand-preventing effect can be realized for a stratum with less serious sand production, and bottom water and side water can be prevented from entering an oil layer for a profile control well or a fracturing well, so that water-controlling and profile control of the oil layer are realized; aiming at reservoirs with three serious types of sand production, namely medium consolidation, weak consolidation and semi-flow sand, the curing liquid is used for reacting with thermosetting epoxy resin to form a precoated sand consolidation body, a stratum architecture is rebuilt, and the sand blocking capability is improved.
The thermosetting epoxy resin layer of the high-temperature-resistant consolidated precoated sand disclosed by the invention can form a stable net structure after a curing reaction with a curing agent. The solidification reaction temperature of the invention is 30-120 ℃, the condition is simple, the invention is easy to occur in thick oil stratum, the consolidation strength of the formed consolidation body is more than 9MPa, and the permeability is more than 1 mu m 2 Has excellent consolidation strength and permeability, and can realize the production of heavy oil wells with serious sand productionThe effects of sand prevention, well cementation, water resistance and oil increase are achieved.
Preferably, the thermosetting epoxy resin curing agent is selected from one of polyamide curing agent, primary amine curing agent, T31 curing agent, anhydride curing agent and imidazole curing agent. The curing reaction principle of the primary amine curing agent is as follows:
preferably, the anhydride curing agent is a phthalic anhydride curing agent.
Preferably, to further increase the reaction speed of curing, the thermosetting epoxy resin curing agent is a primary amine type curing agent, such as JE-4443.
When injecting the high-temperature resistant curable precoated sand and the thermosetting epoxy resin curing agent into the stratum, firstly preparing the thermosetting epoxy resin curing agent into curing liquid. Preferably, the curing liquid is prepared by a method comprising the following steps: taking the mass ratio as curing agent: auxiliary dispersing agent: water =2.8:10:12, stirring for 30min to form a curing liquid, and standing for 24 hours to obtain the product. Preferably, the solvent is methanol and/or ethanol. Preferably, the curing liquid is stirred for 30min before use, so that an excellent curing effect can be ensured.
The high-temperature-resistant consolidated precoated sand disclosed by the invention is solidified by the following liquid in mass ratio: high-temperature resistant curable precoated sand = (7-15): (20-80), uniformly mixing the curing liquid and the high-temperature resistant curable precoated sand, and curing for 24-72 hours at the temperature of 30-120 ℃ to obtain a cured body.
The compressive strength of a consolidated body obtained after the high-temperature resistant consolidated coated sand is solidified can reach more than 9MPa, and the water phase permeability after consolidation is more than 0.5 mu m 2 Oil phase permeability of more than 1 μm 2 The contact angle is greater than 90 deg.. After burning for 2 hours at the high temperature of 350 ℃, the test strength is still kept above 2MPa after cooling, and the contact angle is larger than 90 degrees; placing the consolidation body in a sealed container filled with stratum water, firing at 350 deg.C for 2 hr, cooling, maintaining the test strength above 4MPa, and making the contact angle greater than 90 degree, the consolidation body formed by the high-temperature resistant consolidated precoated sand has high-temperature resistance and water and oil resistance, and can ensure the stability in the application of high-temperature heavy oil well.
Drawings
FIG. 1 is a schematic structural view of a high temperature resistant consolidated precoated sand according to example 1 of the present invention; in the figure, 1-skeleton sand, 2-thermosetting epoxy resin layer and 3-hydrophobic polymer layer;
FIG. 2 is a graph of the appearance of the high temperature resistant consolidated coated sand of example 1 of the present invention;
FIG. 3 is a graph of the appearance of a consolidated artificial core prepared in Experimental example 1 of the present invention;
FIG. 4 is a fracture pressure test curve of a consolidated artificial core prepared in Experimental example 1 of the present invention;
FIG. 5 is a comparison of the appearance of a consolidated artificial core prepared in Experimental example 1 of the present invention before and after high temperature ignition; the left part is before ignition, and the right part is after ignition for 2h at 350 ℃;
FIG. 6 is a fracture pressure test curve after high temperature ignition of a consolidated artificial core prepared in Experimental example 1 of the present invention;
FIG. 7 is a comparison of the appearance of a consolidated artificial core prepared in Experimental example 1 of the present invention before and after firing under formation water immersion conditions; the left part is before firing, and the right part is after firing for 2 hours at 350 ℃ under the condition of stratum water soaking;
FIG. 8 is a fracture pressure test curve of the consolidated artificial core prepared in Experimental example 1 of the present invention after high temperature ignition under formation water immersion.
Detailed Description
The following provides a supplementary explanation of the technical effects of the present invention with reference to specific embodiments.
The raw materials in the following examples and comparative examples are all conventional commercial products, wherein the epoxy resin is E-44, and is purchased from Mooney environmental protection science and technology Hebei Co., ltd; the type of the primary amine curing agent is JE-4443 which is purchased from Hangzhou adhesive company, ltd; the calcium carbonate powder is purchased from Shandong Zhongtian mining industry Co., ltd, and has a nanometer-scale particle size; the sphericity of the quartz sand is more than 0.6.
Example 1
The high-temperature-resistant curable precoated sand of the embodiment has a structural schematic diagram shown in fig. 1, and comprises skeleton sand 1, a thermosetting epoxy resin layer 2 coated on the surface of the skeleton sand 1, and a hydrophobic polymer layer 3 coated on the thermosetting epoxy resin layer 2; the hydrophobic polymer in the hydrophobic polymer layer is obtained by polymerizing 2-acrylamide-2-methylpropanesulfonic acid and acrylamide; the grain size of the skeleton sand is 40/70 meshes; the framework sand is quartz sand, and the mass of the thermosetting epoxy resin is 6.5% of that of the framework sand.
The preparation method of the high-temperature-resistant consolidated precoated sand comprises the following steps:
(1) The quartz sand with the grain size of 40/70 meshes is purified, namely, the quartz sand is washed by water and then dried, so that the mud content is less than 0.5 percent, the micro powder content is less than 1 percent, and the water content is less than 0.2 percent. Weighing 1000g of purified quartz sand, pouring the weighed quartz sand into a sand mixer, heating the quartz sand to 400 ℃, stirring the quartz sand for 120min, and then cooling the quartz sand to 80 ℃ to be used as skeleton sand.
(2) Adding thermosetting epoxy resin E-44 65g (6.5% of the weight of the skeleton sand), stirring and mixing at 80 deg.C for 30min;
(3) Adding 1.95g (3% of the epoxy resin) of calcium carbonate powder, stirring and mixing at 80 ℃ for 30min, cooling to 25 ℃, and compounding the calcium carbonate powder on thermosetting epoxy resin to form resin coated sand;
(4) Adding 36g of hydrochloric acid solution with the mass concentration of 4% to soak the resin coated sand for 3 hours, cleaning the dispersant calcium carbonate powder, and collecting coated particles;
(5) Mixing 118g of 2-acrylamido-2-methylpropanesulfonic acid (MDS) with a solution of 236g of acrylamide (MDS) at a mass concentration of 5%, adjusting the pH to 7, adding 0.35g of ammonium persulfate, carrying out a polymerization reaction at 75 ℃ for 6 hours, and then cooling to obtain a hydrophobic polymer;
(6) Adding 1776mL of acetone organic solvent into the hydrophobic polymer for dilution, mixing with 1060g of the coated particles, stirring and soaking for 4 hours at normal temperature and normal pressure, separating solid particles, and then drying in a 60 ℃ drying oven for 8 hours to enable the hydrophobic polymer to be solidified on the surfaces of the coated particles;
(7) And (5) cooling, discharging and screening to obtain a high-temperature-resistant consolidated precoated sand finished product, wherein the appearance is as shown in figure 2.
Example 2
The high-temperature-resistant curable precoated sand comprises skeleton sand, a thermosetting epoxy resin layer coated on the surface of the skeleton sand and a hydrophobic polymer layer coated on the thermosetting epoxy resin layer; the hydrophobic polymer in the hydrophobic polymer layer is obtained by polymerizing 2-acrylamide-2-methylpropanesulfonic acid and acrylamide; the particle size of the skeleton sand is 20/40 meshes; the framework sand is quartz sand, and the mass of the thermosetting epoxy resin is 5.5% of that of the framework sand.
The preparation method of the high-temperature-resistant consolidated precoated sand comprises the following steps:
(1) The quartz sand with the grain size of 20/40 meshes is purified, namely, the quartz sand is washed by water and then dried, so that the mud content is less than 0.5 percent, the micro powder content is less than 1 percent, and the water content is less than 0.2 percent. Weighing 1000g of purified quartz sand, pouring the weighed quartz sand into a sand mixer, heating the quartz sand to 350 ℃, stirring the quartz sand for 120min, and then cooling the quartz sand to 85 ℃ to be used as skeleton sand.
(2) Adding thermosetting epoxy resin E-44 55g (5.5% of the weight of the skeleton sand), and stirring and mixing at 85 deg.C for 40min;
(3) Adding 1.1g (2% of the epoxy resin) of calcium carbonate powder, stirring and mixing at 85 deg.C for 40min, cooling to below 25 deg.C, and compounding the calcium carbonate powder on thermosetting epoxy resin to form resin coated sand;
(4) Adding 27g of hydrochloric acid solution with the mass concentration of 3% to soak the resin coated sand for 4 hours, cleaning the dispersant calcium carbonate powder, and collecting coated particles;
(5) 344g of 2-acrylamide-2-methylpropanesulfonic acid with the mass concentration of 8% and 184g of acrylamide solution with the mass concentration of 15% are mixed, the pH is adjusted to 8, 0.26g of ammonium persulfate is added to carry out polymerization reaction for 6 hours at the temperature of 75 ℃, and then the temperature is reduced to obtain a hydrophobic polymer;
(6) Adding 1582mL of acetone organic solvent into the hydrophobic polymer for dilution, mixing with 1055g of the coated particles, stirring and soaking for 6 hours at normal temperature and normal pressure, separating solid particles, and then drying in a 50 ℃ drying oven for 12 hours to solidify the hydrophobic polymer on the surfaces of the coated particles;
(7) Cooling, discharging, sieving to obtain the final product, bagging, sealing and storing.
Comparative example 1
The high temperature resistant curable precoated sand of this comparative example was different from example 1 only in that the use of calcium carbonate was omitted, and the result showed that the addition of the thermosetting epoxy resin E-44 resulted in agglomeration after coating and failure to obtain coated particles.
Experimental example 1
This example illustrates a consolidated artificial core prepared from the high temperature resistant consolidated coated sand of example 1.
The consolidated artificial core used in the experimental example is prepared by a method comprising the following steps:
(1) setting the experiment temperature: setting the temperature of the water bath kettle at 50 ℃ and heating to 50 ℃;
(2) preparing a mould: cleaning a core mould with the diameter multiplied by the length of phi 38mm multiplied by 100mm, assembling a base, and putting the base into a 50 ℃ oven;
(3) sample weighing: respectively weighing 80g of the high-temperature resistant consolidated coated sand of example 1 and 15g of the solidification liquid, pouring into a beaker, and uniformly stirring by using a glass rod; the curing liquid is JE-4443, ethanol and water according to the mass ratio of 2.8:10:12 mixing to prepare a homogeneous solution;
(4) filling a sample: after the high-temperature resistant solidifiable precoated sand and the solidifying liquid are uniformly stirred, filling the mixture into a dry forming die for three times and paving the mixture; placing the forming die filled with the sample into a sand sample compaction device each time, compacting for 1 minute under the pressure of 4MPa, taking down the forming die, and continuously adding high-temperature-resistant solidifiable precoated sand mixed with a solidification liquid;
(5) sample pressing: after the forming mold is filled with the high-temperature-resistant solidifiable precoated sand sample, putting the forming mold filled with the sample into a sand sample compaction device, and compacting for 10 minutes under the pressure of 4 MPa;
(6) heating and maintaining a sample: and after the sample is pressed, taking out the forming die sample, putting the forming die sample into a sealing bag, sealing, and then putting the sealing bag into a 50 ℃ water bath pot for curing for 48 hours.
(7) Harvesting the artificial rock core: and after the sample is maintained, removing the base of the forming die, positively pressurizing for 2-3MPa to enable the formed core to move downwards for 10mm, taking down the die, disassembling the die body, and taking out the solidified body. If a damaged surface exists, cutting is needed to obtain the consolidated artificial core, and the appearance is shown in figure 3.
Experimental example 2
This example illustrates a consolidated artificial core prepared from the high temperature resistant consolidated coated sand of example 2.
The consolidated artificial core used in the experimental example is prepared by a method comprising the following steps:
(1) setting the experiment temperature: setting the temperature of the water bath kettle to 50 ℃ and heating to 50 ℃;
(2) preparing a mould: cleaning a core mould with the diameter multiplied by the length of phi 25mm multiplied by 100mm, assembling a base, and putting the base into a 50 ℃ oven;
(3) weighing a sample: respectively weighing 80g of the high-temperature resistant consolidated coated sand of the embodiment 2 and 15g of the solidification liquid, pouring into a beaker, and uniformly stirring by using a glass rod; the curing liquid is JE-4443, methanol and water according to the mass ratio of 2.8:10:12 mixing to prepare a homogeneous solution;
(4) filling a sample: after being uniformly stirred, the high-temperature resistant solidifiable precoated sand and the curing liquid are put into a dry forming die for three times and are paved; placing the forming die filled with the sample into a sand sample compaction device each time, compacting for 1 minute under the pressure of 4MPa, taking down the forming die, and continuously adding high-temperature-resistant solidifiable precoated sand mixed with a solidification liquid;
(5) sample pressing: after the forming mold is filled with the high-temperature-resistant solidifiable precoated sand sample, putting the forming mold filled with the sample into a sand sample compaction device, and compacting for 10 minutes under the pressure of 4 MPa;
(6) heating and maintaining a sample: and after the sample is pressed, taking out the forming die sample, putting the forming die sample into a sealing bag, sealing, and then putting the sealing bag into a 50 ℃ water bath pot for curing for 48 hours.
(7) Harvesting the artificial rock core: and after the sample is maintained, removing the base of the forming die, positively pressurizing for 2-3MPa to enable the formed core to move downwards for 10mm, taking down the die, disassembling the die body, and taking out the solidified body. If a damaged surface exists, cutting is needed to obtain the consolidated artificial core.
Experimental example 3
In this example, the artificial core prepared in example 1 was tested for compressive strength and contact angle under different conditions. During the compression strength test, after the diameter and the length of the consolidated artificial core are rechecked, the artificial core is put into a press machine to measure the crushing pressure of the artificial core, and the compression strength is calculated according to a formula (1):
P＝p 1 /(100A) (1)
in the formula, P is compressive strength, MPa; p is a radical of 1 To the burst pressure, N; a is the cross-sectional area of the artificial rock core in cm 2 。
I) Pre-ignition strength and contact angle testing:
the contact angle of the artificial core of experimental example 1 was measured with a contact angle measuring instrument; the artificial cores of experimental example 1 were respectively put into a press machine to test the burst pressure, wherein the burst pressure test curve of experimental example 1 is shown in fig. 4.
II) testing the strength and the contact angle after high-temperature ignition (dry burning) at 350 ℃:
the artificial rock core of the experimental example 1 is put into a muffle furnace at 350 ℃ to be burned for 2 hours, and the appearance ratio before and after burning is shown in figure 5; after cooling to room temperature, testing the contact angle by using a contact angle measuring instrument; the fired artificial core was then placed in a press and tested for burst pressure, wherein the burst pressure test curve of example 1 is shown in figure 6.
III) testing strength and contact angle after high-temperature ignition (stratum water soaking ignition) at 350 ℃:
the artificial rock core of the experimental example 1 is placed in an iron tank filled with formation water for sealing, and then is placed in a muffle furnace at 350 ℃ for firing for 2 hours so as to simulate the real formation environment of heavy oil well huff and puff exploitation, and the appearance of the formation water before and after soaking and firing is shown in fig. 7; after cooling to room temperature, testing the contact angle by using a contact angle measuring instrument; and then putting the burned artificial rock cores into a press respectively, and testing the fracture pressure, wherein the test curve of the fracture pressure after burning is shown in figure 8.
Experimental example 4
The artificial core prepared in experimental example 2 was tested for compressive strength and contact angle under different conditions. During the compression strength test, after the diameter and the length of the consolidated artificial core are rechecked, the consolidated artificial core is put into a press machine to measure the crushing pressure of the artificial core, and the compression strength is calculated according to a formula (1):
P＝p 1 /(100A) (1)
in the formula, P is compressive strength, MPa; p is a radical of 1 To the burst pressure, N; a is the cross section area of the artificial rock core in cm 2 。
I) Pre-ignition strength and contact angle testing:
the contact angle of the artificial core of experimental example 2 was measured with a contact angle measuring instrument; the artificial cores of experimental example 2 were placed in a press, respectively, and the respective rupture pressures were tested.
II) testing the strength and the contact angle after high-temperature ignition (dry burning) at 350 ℃:
placing the artificial rock core of the experimental example 2 into a muffle furnace at 350 ℃ for firing for 2 hours, cooling to room temperature, and testing the contact angle of the artificial rock core by using a contact angle measuring instrument; and then putting the burned artificial rock cores into a press machine respectively, and testing the fracture pressure.
III) testing strength and contact angle after high-temperature ignition (stratum water soaking ignition) at 350 ℃:
the artificial rock core of the experimental example 2 is placed in an iron tank filled with formation water for sealing, and then is placed in a muffle furnace at 350 ℃ for firing for 2 hours so as to simulate the real formation environment of huff and puff exploitation of a heavy oil well; after cooling to room temperature, testing the contact angle by using a contact angle measuring instrument; and then putting the burned artificial rock cores into a press machine respectively, and testing the fracture pressure. The results of the strength and contact angle tests of experimental example 3 and experimental example 4 are shown in table 1 below.
TABLE 1 results of strength and contact angle measurements of artificial cores
Claims (9)
1. The high-temperature-resistant consolidated precoated sand is characterized in that: the sand comprises skeleton sand, a thermosetting epoxy resin layer coated on the surface of the skeleton sand and a hydrophobic polymer layer coated on the thermosetting epoxy resin layer; the hydrophobic polymer in the hydrophobic polymer layer is obtained by polymerizing 2-acrylamide-2-methylpropanesulfonic acid and acrylamide.
2. The high temperature resistant consolidated coated sand of claim 1, wherein: the thermosetting epoxy resin in the thermosetting epoxy resin layer is bisphenol A diglycidyl ether; the epoxy value of the thermosetting epoxy resin is 0.41-0.47.
3. The high temperature resistant consolidated coated sand of claim 1, wherein: the particle size of the skeleton sand is 40-120 meshes; the skeleton sand is quartz sand.
4. The high temperature resistant consolidated coated sand of any of claims 1-3, wherein: the mass ratio of the 2-acrylamide-2-methyl propane sulfonic acid to the acrylamide is (5-8) to (10-15).
5. The method of preparing the high temperature resistant consolidated coated sand of any of claims 1-4, wherein: the method comprises the following steps:
1) Mixing the skeleton sand with thermosetting epoxy resin to coat the thermosetting epoxy resin on the surface of the skeleton sand, and then stirring and mixing the skeleton sand with a dispersing agent to obtain resin coated sand; the dispersing agent is calcium carbonate powder;
2) Carrying out acid washing on the resin coated sand to remove the dispersant, and obtaining coated particles;
3) And (3) soaking the coated particles in a hydrophobic polymer solution, and drying to obtain the coating.
6. The method of preparing high temperature resistant consolidated coated sand of claim 5, wherein: the mass of the thermosetting epoxy resin in the thermosetting epoxy resin layer is 5.5-6.5% of that of the skeleton sand; the mass of the calcium carbonate powder is 2.0-3.0% of that of the thermosetting epoxy resin.
7. The method of making high temperature resistant consolidated coated sand of claim 5 or 6, wherein: the hydrophobic polymer solution is obtained by diluting a hydrophobic polymer by 4-6 times with acetone; in the step 3), the mass ratio of the coated particles to the hydrophobic polymer solution is 1:2, the soaking time is 4-6 h.
8. The method of preparing high temperature resistant consolidated coated sand of claim 5, wherein: in the step 3), the hydrophobic polymer is obtained by polymerizing 2-acrylamido-2-methylpropanesulfonic acid and acrylamide, and the mass ratio of the 2-acrylamido-2-methylpropanesulfonic acid to the acrylamide is (5-8) to (10-15).
9. The method of preparing the high temperature resistant consolidated coated sand of claim 5, wherein: and (2) mixing the skeleton sand and thermosetting epoxy resin in the step 1), stirring and mixing at 80-85 ℃, and cooling to below 25 ℃ after stirring and mixing to obtain the resin coated sand.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210613790.5A CN115232608A (en) | 2022-05-31 | 2022-05-31 | High-temperature-resistant consolidated precoated sand and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210613790.5A CN115232608A (en) | 2022-05-31 | 2022-05-31 | High-temperature-resistant consolidated precoated sand and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN115232608A true CN115232608A (en) | 2022-10-25 |
Family
ID=83669369
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210613790.5A Pending CN115232608A (en) | 2022-05-31 | 2022-05-31 | High-temperature-resistant consolidated precoated sand and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115232608A (en) |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5010953A (en) * | 1990-01-02 | 1991-04-30 | Texaco Inc. | Sand consolidation methods |
| US20050284632A1 (en) * | 2004-06-29 | 2005-12-29 | Dalrymple Eldon D | Methods useful for controlling fluid loss during sand control operations |
| CN103194205A (en) * | 2013-04-12 | 2013-07-10 | 中国石油天然气股份有限公司 | Heat-resistant high-strength precoated sand fracturing propping agent and preparation method thereof |
| CN104449624A (en) * | 2014-11-24 | 2015-03-25 | 武汉工程大学 | Novel sand control agent for high-temperature sand control in steam huff-puff oil well |
| CA2993264A1 (en) * | 2015-08-26 | 2017-03-02 | Halliburton Energy Services, Inc. | Sugar based epoxy resins with enhanced properties for sand consolidation in subterranean formations |
| CN109370560A (en) * | 2018-10-25 | 2019-02-22 | 中国石油天然气股份有限公司 | One heavy metal species mineralizer class temperature consolidates coated sand and the preparation method and application thereof |
| CN111607374A (en) * | 2020-04-14 | 2020-09-01 | 中国石油化工股份有限公司 | Low-temperature curing oil-permeable water-blocking precoated sand and preparation method thereof |
| CN114181684A (en) * | 2021-12-15 | 2022-03-15 | 中国石油化工股份有限公司 | Water-blocking oil-permeable precoated sand, preparation method thereof and chemical sand prevention system |
-
2022
- 2022-05-31 CN CN202210613790.5A patent/CN115232608A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5010953A (en) * | 1990-01-02 | 1991-04-30 | Texaco Inc. | Sand consolidation methods |
| US20050284632A1 (en) * | 2004-06-29 | 2005-12-29 | Dalrymple Eldon D | Methods useful for controlling fluid loss during sand control operations |
| CN103194205A (en) * | 2013-04-12 | 2013-07-10 | 中国石油天然气股份有限公司 | Heat-resistant high-strength precoated sand fracturing propping agent and preparation method thereof |
| CN104449624A (en) * | 2014-11-24 | 2015-03-25 | 武汉工程大学 | Novel sand control agent for high-temperature sand control in steam huff-puff oil well |
| CA2993264A1 (en) * | 2015-08-26 | 2017-03-02 | Halliburton Energy Services, Inc. | Sugar based epoxy resins with enhanced properties for sand consolidation in subterranean formations |
| CN109370560A (en) * | 2018-10-25 | 2019-02-22 | 中国石油天然气股份有限公司 | One heavy metal species mineralizer class temperature consolidates coated sand and the preparation method and application thereof |
| CN111607374A (en) * | 2020-04-14 | 2020-09-01 | 中国石油化工股份有限公司 | Low-temperature curing oil-permeable water-blocking precoated sand and preparation method thereof |
| CN114181684A (en) * | 2021-12-15 | 2022-03-15 | 中国石油化工股份有限公司 | Water-blocking oil-permeable precoated sand, preparation method thereof and chemical sand prevention system |
Non-Patent Citations (1)
| Title |
|---|
| 曲占庆;曲冠政;张永昌;何利敏;王冰;: "控水防砂剂室内评价及现场应用研究", 科学技术与工程 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103409121B (en) | A kind of water-soluble pressure break turns to temporary plugging agent and preparation method thereof | |
| CN104893707A (en) | Self-suspension proppant for hydraulic fracturing and preparation method thereof | |
| CN109777387B (en) | Repeated fracturing temporary plugging agent and preparation method and application thereof | |
| CN108033710A (en) | A kind of Ultralight overlay film proppant and preparation method thereof | |
| CN110079295B (en) | Curable proppant and preparation method and application thereof | |
| CN106244136B (en) | A kind of curable sand control proppant and preparation method thereof | |
| CN105400503B (en) | A kind of reservoir profile water shutoff agent of resisting high temperature, high salt and preparation method thereof | |
| CN105542739B (en) | A kind of sand control coated sand and preparation method thereof | |
| CN108976366B (en) | Hydrophobic film-coated propping agent and preparation method and application thereof | |
| CN111548779B (en) | Temporary plugging agent and preparation method thereof | |
| CN114716984B (en) | Cementing and plugging type wall fixing agent for water-based drilling fluid and preparation method and application thereof | |
| CN104449655A (en) | Fracture-cavern type oil reservoir filtrate reducer composition and fracture-cavern type oil reservoir filtrate reducing method | |
| CN106675548A (en) | Self-suspension propping agent and preparation method thereof | |
| CN111285642A (en) | Plugging agent, preparation method and application thereof | |
| CN114181684B (en) | Water-blocking oil-permeable precoated sand, preparation method thereof and chemical sand prevention system | |
| CN105505372A (en) | Sand prevention and water reduction proppant particles and preparing method thereof | |
| CN109370560B (en) | Heavy metal mineralized substance warm-curing resin precoated sand and preparation method and application thereof | |
| CN101200632A (en) | Method and technique for preparing low-density propping agent | |
| CN104311719A (en) | Chemical bonding type relative phase modifier suitable for high-mineralization-degree oil reservoir | |
| CN115232608A (en) | High-temperature-resistant consolidated precoated sand and preparation method thereof | |
| CN111607374B (en) | Low-temperature curing oil-permeable water-blocking precoated sand and preparation method thereof | |
| CN110229651B (en) | Resin plugging agent for repairing cement annulus cracks and preparation method thereof | |
| CN112282722A (en) | Low-density organic water-control proppant and preparation method thereof | |
| CN115074108B (en) | Coal bed gas fracturing propping agent and polymer fracturing liquid system | |
| CN106634919B (en) | A kind of containing consolidated sand system and preparation method thereof and application method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |