CN119842027B - A high-temperature resistant temporary plugging agent for oil fields and its preparation method - Google Patents
A high-temperature resistant temporary plugging agent for oil fields and its preparation methodInfo
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- CN119842027B CN119842027B CN202510337131.7A CN202510337131A CN119842027B CN 119842027 B CN119842027 B CN 119842027B CN 202510337131 A CN202510337131 A CN 202510337131A CN 119842027 B CN119842027 B CN 119842027B
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F290/00—Macromolecular compounds obtained by polymerising monomers on to polymers modified by introduction of aliphatic unsaturated end or side groups
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Abstract
本发明公开了一种油田用耐高温暂堵剂及其制备方法，该暂堵剂以丙烯酰胺、丙烯酸、2‑丙烯酰胺‑2‑甲基丙磺酸和蓖麻油为反应原料，与改性交联剂交联，并与改性填料共混聚合，制得耐高温暂堵剂，该暂堵剂的分子结构为网格状聚丙烯酰胺，聚丙烯酰胺分子链上含有酰胺基团、磺酸基团和羧基，酰胺基团为不带电基团，不易受到高矿化度底层水影响，磺酸基团能够增加暂堵剂的抗盐性能，羧基能够与水中的氢离子发生络合，进而使得网格分子水化膨胀，侧链含有聚硅氧烷链段以及长链烷基，使得该暂堵剂在高温环境仍然能够正常使用，长链烷基形成疏水微区，能够与地层岩石的疏水表面吸附，使得暂堵剂在施工过程中保持稳定状态。The invention discloses a high-temperature resistant temporary plugging agent for oil fields and a preparation method thereof. The temporary plugging agent uses acrylamide, acrylic acid, 2-acrylamide-2-methylpropane sulfonic acid and castor oil as reaction raw materials, cross-links with a modified cross-linking agent, and is blended and polymerized with a modified filler to prepare the high-temperature resistant temporary plugging agent. The molecular structure of the temporary plugging agent is a grid-shaped polyacrylamide. The polyacrylamide molecular chain contains an amide group, a sulfonic acid group and a carboxyl group. The amide group is an uncharged group and is not easily affected by high-mineralization bottom water. The sulfonic acid group can increase the salt resistance of the temporary plugging agent. The carboxyl group can complex with hydrogen ions in water, thereby causing the grid molecules to hydrate and expand. The side chain contains a polysiloxane segment and a long-chain alkyl group, so that the temporary plugging agent can still be used normally in a high-temperature environment. The long-chain alkyl group forms a hydrophobic microdomain and can be adsorbed to the hydrophobic surface of the formation rock, so that the temporary plugging agent remains stable during construction.
Description
Technical Field
The invention relates to the technical field of temporary plugging agent preparation, in particular to a high-temperature-resistant temporary plugging agent for an oil field and a preparation method thereof.
Background
In the process of drilling, well completion and other operations, when external fluid enters a reservoir, a series of adverse effects such as solid phase migration, clay expansion, precipitation blocking pore roar caused by incompatible fluid and the like can be caused, so that the permeability of the reservoir near-wellbore zone is reduced, the productivity of an oil layer is reduced, temporary blocking is shielded by a temporary blocking agent, which is an easy-to-implement oil and gas layer protection technology, is widely used, and the temporary blocking agent is a material capable of temporarily reducing the permeability of the reservoir and can effectively inhibit working fluid from entering a non-target reservoir. As reservoir depth increases, formation temperature increases. When developing deep-ultra-deep oil and gas resources, the conventional temporary plugging agent is difficult to have the effect of high temperature resistance at the same time, so that the temporary plugging agent fails, and the plugging effect cannot be achieved.
Disclosure of Invention
The invention aims to provide a high-temperature-resistant temporary plugging agent for an oil field and a preparation method thereof, which solve the problems of poor stability, poor pore and crack plugging effect and insufficient gel strength at the present stage under the high temperature condition.
The aim of the invention can be achieved by the following technical scheme:
the preparation method of the high-temperature-resistant temporary plugging agent for the oil field specifically comprises the following steps:
step A1, uniformly mixing tetramethyl cyclotetrasiloxane, 1-octene, chloroplatinic acid and DMF, introducing nitrogen for protection, and reacting for 3-5 hours under the condition that the rotating speed is 120-150r/min and the temperature is 70-80 ℃ to obtain a modified monomer;
A2, mixing octamethyl cyclotetrasiloxane, modified monomer, tetramethyl divinyl disiloxane, tetramethyl ammonium hydroxide and dimethyl sulfoxide, introducing nitrogen for protection, and reacting for 10-12 hours under the condition that the rotating speed is 120-150r/min and the temperature is 90-95 ℃ to prepare a modified cross-linking agent;
And step A3, uniformly mixing acrylamide, acrylic acid, 2-acrylamide-2-methylpropanesulfonic acid, castor oil and DMF, adding a modified cross-linking agent and a modified filler under the conditions of the rotating speed of 150-200r/min, the temperature of 20-25 ℃ and the pH value of neutrality, stirring for 1-1.5h, adding dicumyl peroxide, heating to 120-125 ℃ and reacting for 2-3h to obtain the high-temperature-resistant temporary plugging agent for the oil field.
Further, the molar ratio of the tetramethyl cyclotetrasiloxane to the 1-octene in the step A1 is 1:1, and the dosage of chloroplatinic acid is 1 per mill of the mass of the 1-octene.
Further, the molar ratio of octamethyl cyclotetrasiloxane, modified monomer, tetramethyl divinyl disiloxane and tetramethyl ammonium hydroxide in the step A2 is 1.6:0.8:1:2.
Further, the molar ratio of the acrylamide to the acrylic acid to the 2-acrylamide-2-methylpropanesulfonic acid to the castor oil in the step A3 is 15:1:4:2, the dosage of the modified cross-linking agent is 4 per mill of the sum of the mass of the acrylamide, the acrylic acid, the 2-acrylamide-2-methylpropanesulfonic acid and the castor oil, the dosage of the modified filler is 5 per mill of the sum of the mass of the acrylamide, the acrylic acid, the 2-acrylamide-2-methylpropanesulfonic acid and the castor oil, and the dosage of the dicumyl peroxide is 3 per mill of the sum of the mass of the acrylamide, the acrylic acid, the 2-acrylamide-2-methylpropanesulfonic acid and the castor oil.
Further, the modified filler is prepared by the following steps:
Dispersing calcium carbonate in ethanol, stirring and adding KH550 and deionized water at the rotating speed of 200-300r/min and the temperature of 60-70 ℃ for reacting for 2-3 hours to obtain pretreated calcium carbonate, uniformly mixing the pretreated calcium carbonate, 3, 4-epoxy-1-butene and DMF, and reacting for 2-3 hours at the rotating speed of 200-300r/min, the temperature of 40-50 ℃ and the pH value of 11-12 to obtain modified calcium carbonate;
Step B2, uniformly mixing caprolactone, modified calcium carbonate, stannous octoate and DMF, introducing nitrogen for protection, reacting for 20-25 hours at the rotation speed of 150-200r/min and the temperature of 120-125 ℃ to obtain a precursor, uniformly mixing cellulose, chlorinated 1-butyl-3-methylimidazole and DMF, introducing nitrogen for protection, stirring and adding 2-bromo-2-methylpropanoyl bromide at the rotation speed of 120-150r/min and the temperature of 0-3 ℃ for reacting for 1-2 hours, heating to 20-25 ℃ and continuing to react for 3-5 hours to obtain pretreated cellulose;
and B3, dispersing the pretreated cellulose in DMF, introducing nitrogen for protection, stirring and adding thiourea at the rotating speed of 150-200r/min and the temperature of 75-80 ℃, reacting for 20-25h, removing DMF, adding sodium hydroxide solution, reacting for 1-1.5h at the temperature of 102-105 ℃, regulating the pH value to 2-3, preparing the sulfhydryl cellulose, uniformly mixing the sulfhydryl cellulose, the precursor, the benzophenone and the ethanol, and reacting for 5-10min under the irradiation of 365nm ultraviolet light, thus preparing the modified filler.
Further, KH550 was used in an amount of 1% by mass of calcium carbonate in the molar ratio of amino groups to 3, 4-epoxy-1-butene on the pretreated calcium carbonate of 1:2.
Further, the mass ratio of caprolactone to modified calcium carbonate to stannous octoate in the step B2 is 100:10:1, and the dosage ratio of cellulose to 1g:20g to 12mL of 1-butyl-3-methylimidazole chloride to 2-bromo-2-methylpropionamide.
Further, the dosage ratio of the pretreated cellulose to the thiourea to the sodium hydroxide solution in the step B3 is 0.5g:25mmol:100mL, the mass fraction of the sodium hydroxide solution is 1.5%, the mass ratio of the sulfhydryl cellulose to the precursor is 5:1, and the dosage of the benzophenone is5 per mill of that of the modified calcium carbonate.
The invention has the beneficial effects that the high-temperature-resistant temporary plugging agent for the oil field disclosed by the invention takes acrylamide, acrylic acid, 2-acrylamide-2-methylpropanesulfonic acid and castor oil as reaction raw materials, a modified crosslinking agent is crosslinked and is mixed with modified fillers for polymerization to prepare the high-temperature-resistant temporary plugging agent, the modified crosslinking agent takes tetramethyl cyclotetrasiloxane and 1-octene as raw materials for reaction, so that Si-H bonds on the tetramethyl cyclotetrasiloxane react with double bonds on 1-octene to prepare a modified monomer, the modified monomer and octamethyl cyclotetrasiloxane are subjected to ring-opening condensation, and then are treated by tetramethyl divinyl disiloxane to form double bond end caps, so that the modified crosslinking agent is prepared.
The modified filler is prepared by using calcium carbonate as a raw material and using KH550 to treat the surface of the modified filler so as to graft amino groups, preparing pretreated calcium carbonate, reacting the pretreated calcium carbonate with 3, 4-epoxy-1-butene to enable the amino groups on the surface of the pretreated calcium carbonate and the epoxy groups on the 3, 4-epoxy-1-butene to react to form hydroxyl groups, preparing modified calcium carbonate, coating polycaprolactone and the modified calcium carbonate on the surface of the modified calcium carbonate under the action of stannous octoate to prepare a precursor, treating cellulose with 2-bromo-2-methylpropanoyl bromide to enable hydroxyl groups at C6 position on cellulose molecules to react with acyl bromide on 2-bromo-2-methylpropanoyl bromide to prepare pretreated cellulose, treating the pretreated cellulose with thiourea to enable bromine atom sites on the pretreated cellulose to be converted into mercapto groups, preparing mercapto cellulose, reacting the mercapto cellulose with the precursor under the irradiation of ultraviolet light to enable the mercapto groups on the mercapto cellulose and the double bond on the precursor to graft.
The molecular structure of the temporary plugging agent is latticed polyacrylamide, an amide group, a sulfonic acid group and a carboxyl are contained on a polyacrylamide molecular chain, the amide group is an uncharged group and is not easily influenced by high-mineralization bottom water, the sulfonic acid group can increase the salt resistance of the temporary plugging agent, the carboxyl can be complexed with hydrogen ions in water, so that the latticed molecule is hydrated and expanded, a side chain contains a polysiloxane chain segment and a long-chain alkyl, the temporary plugging agent can still be normally used in a high-temperature environment, the long-chain alkyl forms a hydrophobic micro-area and can be adsorbed with the hydrophobic surface of stratum rock, the hydroxyl content in molecules is increased by adding castor oil, the water absorbability of the temporary plugging agent is further improved, the temporary plugging agent can be rapidly expanded and plug a high-permeability area in the stratum, cellulose on the surface of a modified filler is also water-absorbed and can squeeze adjacent modified filler, and the temporary plugging agent can keep a stable state in a construction process.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Embodiment 1, a preparation method of a high-temperature-resistant temporary plugging agent for an oil field specifically comprises the following steps:
step A1, uniformly mixing tetramethyl cyclotetrasiloxane, 1-octene, chloroplatinic acid and DMF, introducing nitrogen for protection, and reacting for 3 hours under the condition of 120r/min of rotating speed and 70 ℃ to obtain a modified monomer;
A2, mixing octamethyl cyclotetrasiloxane, modified monomer, tetramethyl divinyl disiloxane, tetramethyl ammonium hydroxide and dimethyl sulfoxide, introducing nitrogen for protection, and reacting for 10 hours under the condition that the rotating speed is 120r/min and the temperature is 90 ℃ to obtain a modified crosslinking agent;
and step A3, uniformly mixing acrylamide, acrylic acid, 2-acrylamide-2-methylpropanesulfonic acid, castor oil and DMF, adding a modified cross-linking agent and a modified filler under the conditions of 150r/min, 20 ℃ and neutral pH, stirring for 1h, adding dicumyl peroxide, heating to 120 ℃ and reacting for 2h to obtain the high-temperature-resistant temporary plugging agent for the oil field.
The molar ratio of the tetramethyl cyclotetrasiloxane to the 1-octene in the step A1 is 1:1, and the dosage of the chloroplatinic acid is 1 per mill of the mass of the 1-octene.
The molar ratio of the octamethyl cyclotetrasiloxane, the modified monomer, the tetramethyl divinyl disiloxane and the tetramethyl ammonium hydroxide in the step A2 is 1.6:0.8:1:2.
The mol ratio of the acrylamide to the acrylic acid to the 2-acrylamide-2-methylpropanesulfonic acid to the castor oil in the step A3 is 15:1:4:2, the dosage of the modified cross-linking agent is 4 per mill of the sum of the mass of the acrylamide, the acrylic acid, the 2-acrylamide-2-methylpropanesulfonic acid and the castor oil, the dosage of the modified filler is 5 per mill of the sum of the mass of the acrylamide, the acrylic acid, the 2-acrylamide-2-methylpropanesulfonic acid and the castor oil, and the dosage of the dicumyl peroxide is 3 per mill of the sum of the mass of the acrylamide, the acrylic acid, the 2-acrylamide-2-methylpropanesulfonic acid and the castor oil.
The modified filler is prepared by the following steps:
Dispersing calcium carbonate in ethanol, stirring and adding KH550 and deionized water under the conditions of the rotating speed of 200r/min and the temperature of 60 ℃ for reaction for 2 hours to obtain pretreated calcium carbonate, uniformly mixing the pretreated calcium carbonate, 3, 4-epoxy-1-butene and DMF, and reacting for 2 hours under the conditions of the rotating speed of 200r/min, the temperature of 40 ℃ and the pH value of 11 to obtain modified calcium carbonate;
Step B2, uniformly mixing caprolactone, modified calcium carbonate, stannous octoate and DMF, introducing nitrogen for protection, reacting for 20 hours at the rotation speed of 150r/min and the temperature of 120 ℃, uniformly mixing cellulose, chlorinated 1-butyl-3-methylimidazole and DMF, introducing nitrogen for protection, stirring and adding 2-bromo-2-methylpropanoyl bromide at the rotation speed of 120r/min and the temperature of 0 ℃, reacting for 1 hour, heating to 20 ℃, and continuing to react for 3 hours to obtain pretreated cellulose;
And B3, dispersing the pretreated cellulose in DMF, introducing nitrogen for protection, stirring and adding thiourea at the rotating speed of 150r/min and the temperature of 75 ℃, carrying out reaction for 20 hours, removing DMF, adding sodium hydroxide solution, carrying out reaction for 1 hour at the temperature of 102 ℃, regulating the pH value to 2, obtaining the sulfhydryl cellulose, uniformly mixing the sulfhydryl cellulose, the precursor, the diphenyl ketone and the ethanol, and carrying out reaction for 5 minutes under the irradiation of 365nm ultraviolet light, thus obtaining the modified filler.
KH550 is used in the step B1 in an amount of 1% of the mass of the calcium carbonate, and the molar ratio of amino groups to 3, 4-epoxy-1-butene on the pretreated calcium carbonate is 1:2.
The mass ratio of caprolactone to modified calcium carbonate to stannous octoate in the step B2 is 100:10:1, and the dosage ratio of cellulose to 1g to 20g to 12mL of 1-butyl-3-methylimidazole chloride to 2-bromo-2-methylpropionyl bromide.
The dosage ratio of the pretreated cellulose to the thiourea to the sodium hydroxide solution in the step B3 is 0.5 g/25 mmol/100 mL, the mass fraction of the sodium hydroxide solution is 1.5%, the mass ratio of the sulfhydryl cellulose to the precursor is 5:1, and the dosage of the diphenyl ketone is 5%o of that of the modified calcium carbonate.
Embodiment 2, a preparation method of a high temperature resistant temporary plugging agent for oil fields, specifically comprises the following steps:
Step A1, uniformly mixing tetramethyl cyclotetrasiloxane, 1-octene, chloroplatinic acid and DMF, introducing nitrogen for protection, and reacting for 4 hours under the condition that the rotating speed is 120r/min and the temperature is 75 ℃ to obtain a modified monomer;
A2, mixing octamethyl cyclotetrasiloxane, modified monomer, tetramethyl divinyl disiloxane, tetramethyl ammonium hydroxide and dimethyl sulfoxide, introducing nitrogen for protection, and reacting for 11 hours under the condition that the rotating speed is 120r/min and the temperature is 95 ℃ to obtain a modified crosslinking agent;
And step A3, uniformly mixing acrylamide, acrylic acid, 2-acrylamide-2-methylpropanesulfonic acid, castor oil and DMF, adding a modified cross-linking agent and a modified filler under the conditions of 150r/min, 25 ℃ and neutral pH, stirring for 1.3 hours, adding dicumyl peroxide, heating to 125 ℃, and reacting for 2 hours to obtain the high-temperature-resistant temporary plugging agent for the oil field.
The molar ratio of the tetramethyl cyclotetrasiloxane to the 1-octene in the step A1 is 1:1, and the dosage of the chloroplatinic acid is 1 per mill of the mass of the 1-octene.
The molar ratio of the octamethyl cyclotetrasiloxane, the modified monomer, the tetramethyl divinyl disiloxane and the tetramethyl ammonium hydroxide in the step A2 is 1.6:0.8:1:2.
The mol ratio of the acrylamide to the acrylic acid to the 2-acrylamide-2-methylpropanesulfonic acid to the castor oil in the step A3 is 15:1:4:2, the dosage of the modified cross-linking agent is 4 per mill of the sum of the mass of the acrylamide, the acrylic acid, the 2-acrylamide-2-methylpropanesulfonic acid and the castor oil, the dosage of the modified filler is 5 per mill of the sum of the mass of the acrylamide, the acrylic acid, the 2-acrylamide-2-methylpropanesulfonic acid and the castor oil, and the dosage of the dicumyl peroxide is 3 per mill of the sum of the mass of the acrylamide, the acrylic acid, the 2-acrylamide-2-methylpropanesulfonic acid and the castor oil.
The modified filler is prepared by the following steps:
dispersing calcium carbonate in ethanol, stirring and adding KH550 and deionized water under the conditions of the rotating speed of 300r/min and the temperature of 65 ℃ for 2 hours to obtain pretreated calcium carbonate, uniformly mixing the pretreated calcium carbonate, 3, 4-epoxy-1-butene and DMF, and reacting for 3 hours under the conditions of the rotating speed of 300r/min, the temperature of 45 ℃ and the pH value of 11 to obtain modified calcium carbonate;
step B2, uniformly mixing caprolactone, modified calcium carbonate, stannous octoate and DMF, introducing nitrogen for protection, reacting for 20 hours at the rotation speed of 150r/min and the temperature of 125 ℃ to obtain a precursor, uniformly mixing cellulose, chlorinated 1-butyl-3-methylimidazole and DMF, introducing nitrogen for protection, stirring and adding 2-bromo-2-methylpropanoyl bromide at the rotation speed of 150r/min and the temperature of 0 ℃ for reacting for 2 hours, heating to 20 ℃, and continuing to react for 4 hours to obtain pretreated cellulose;
And B3, dispersing the pretreated cellulose in DMF, introducing nitrogen for protection, stirring and adding thiourea at the rotating speed of 150r/min and the temperature of 80 ℃, carrying out reaction for 20 hours, removing DMF, adding sodium hydroxide solution, carrying out reaction for 1.5 hours at the temperature of 103 ℃, regulating the pH value to 2, preparing the sulfhydryl cellulose, uniformly mixing the sulfhydryl cellulose, the precursor, the diphenyl ketone and the ethanol, and carrying out reaction for 8 minutes under the irradiation of 365nm ultraviolet light, thus preparing the modified filler.
KH550 is used in the step B1 in an amount of 1% of the mass of the calcium carbonate, and the molar ratio of amino groups to 3, 4-epoxy-1-butene on the pretreated calcium carbonate is 1:2.
The mass ratio of caprolactone to modified calcium carbonate to stannous octoate in the step B2 is 100:10:1, and the dosage ratio of cellulose to 1g to 20g to 12mL of 1-butyl-3-methylimidazole chloride to 2-bromo-2-methylpropionyl bromide.
The dosage ratio of the pretreated cellulose to the thiourea to the sodium hydroxide solution in the step B3 is 0.5 g/25 mmol/100 mL, the mass fraction of the sodium hydroxide solution is 1.5%, the mass ratio of the sulfhydryl cellulose to the precursor is 5:1, and the dosage of the diphenyl ketone is 5%o of that of the modified calcium carbonate.
Embodiment 3, a preparation method of a high-temperature-resistant temporary plugging agent for oil fields, specifically comprises the following steps:
Step A1, uniformly mixing tetramethyl cyclotetrasiloxane, 1-octene, chloroplatinic acid and DMF, introducing nitrogen for protection, and reacting for 5 hours under the condition of the rotating speed of 150r/min and the temperature of 80 ℃ to obtain a modified monomer;
A2, mixing octamethyl cyclotetrasiloxane, modified monomer, tetramethyl divinyl disiloxane, tetramethyl ammonium hydroxide and dimethyl sulfoxide, introducing nitrogen for protection, and reacting for 12 hours under the condition of the rotating speed of 150r/min and the temperature of 95 ℃ to obtain a modified cross-linking agent;
And step A3, uniformly mixing acrylamide, acrylic acid, 2-acrylamide-2-methylpropanesulfonic acid, castor oil and DMF, adding a modified cross-linking agent and a modified filler under the conditions of 200r/min rotational speed, 25 ℃ and neutral pH, stirring for 1.5h, adding dicumyl peroxide, heating to 125 ℃, and reacting for 3h to obtain the high-temperature-resistant temporary plugging agent for the oil field.
The molar ratio of the tetramethyl cyclotetrasiloxane to the 1-octene in the step A1 is 1:1, and the dosage of the chloroplatinic acid is 1 per mill of the mass of the 1-octene.
The molar ratio of the octamethyl cyclotetrasiloxane, the modified monomer, the tetramethyl divinyl disiloxane and the tetramethyl ammonium hydroxide in the step A2 is 1.6:0.8:1:2.
The mol ratio of the acrylamide to the acrylic acid to the 2-acrylamide-2-methylpropanesulfonic acid to the castor oil in the step A3 is 15:1:4:2, the dosage of the modified cross-linking agent is 4 per mill of the sum of the mass of the acrylamide, the acrylic acid, the 2-acrylamide-2-methylpropanesulfonic acid and the castor oil, the dosage of the modified filler is 5 per mill of the sum of the mass of the acrylamide, the acrylic acid, the 2-acrylamide-2-methylpropanesulfonic acid and the castor oil, and the dosage of the dicumyl peroxide is 3 per mill of the sum of the mass of the acrylamide, the acrylic acid, the 2-acrylamide-2-methylpropanesulfonic acid and the castor oil.
The modified filler is prepared by the following steps:
Dispersing calcium carbonate in ethanol, stirring and adding KH550 and deionized water under the conditions of the rotating speed of 300r/min and the temperature of 70 ℃ for reaction for 3 hours to obtain pretreated calcium carbonate, uniformly mixing the pretreated calcium carbonate, 3, 4-epoxy-1-butene and DMF, and reacting for 3 hours under the conditions of the rotating speed of 300r/min, the temperature of 50 ℃ and the pH value of 12 to obtain modified calcium carbonate;
Step B2, uniformly mixing caprolactone, modified calcium carbonate, stannous octoate and DMF, introducing nitrogen for protection, reacting for 25 hours at the rotation speed of 200r/min and the temperature of 125 ℃ to obtain a precursor, uniformly mixing cellulose, chlorinated 1-butyl-3-methylimidazole and DMF, introducing nitrogen for protection, stirring and adding 2-bromo-2-methylpropanoyl bromide at the rotation speed of 150r/min and the temperature of 3 ℃ for reacting for 2 hours, heating to 25 ℃, and continuing to react for 5 hours to obtain pretreated cellulose;
and B3, dispersing the pretreated cellulose in DMF, introducing nitrogen for protection, stirring and adding thiourea at the rotating speed of 200r/min and the temperature of 80 ℃, carrying out reaction for 25 hours, removing DMF, adding sodium hydroxide solution, carrying out reaction for 1.5 hours at the temperature of 105 ℃, regulating the pH value to 3, preparing the sulfhydryl cellulose, uniformly mixing the sulfhydryl cellulose, the precursor, the diphenyl ketone and the ethanol, and carrying out reaction for 10 minutes under the irradiation of 365nm ultraviolet light, thus preparing the modified filler.
KH550 is used in the step B1 in an amount of 1% of the mass of the calcium carbonate, and the molar ratio of amino groups to 3, 4-epoxy-1-butene on the pretreated calcium carbonate is 1:2.
The mass ratio of caprolactone to modified calcium carbonate to stannous octoate in the step B2 is 100:10:1, and the dosage ratio of cellulose to 1g to 20g to 12mL of 1-butyl-3-methylimidazole chloride to 2-bromo-2-methylpropionyl bromide.
The dosage ratio of the pretreated cellulose to the thiourea to the sodium hydroxide solution in the step B3 is 0.5 g/25 mmol/100 mL, the mass fraction of the sodium hydroxide solution is 1.5%, the mass ratio of the sulfhydryl cellulose to the precursor is 5:1, and the dosage of the diphenyl ketone is 5%o of that of the modified calcium carbonate.
Comparative example 1, in which castor oil was not added as compared with example 1, the rest of the procedure was the same.
Comparative example 2 this comparative example uses N, N-methylenebisacrylamide instead of the modified crosslinker as compared to example 1.
Comparative example 3, in which no mercaptocellulose was added as compared with example 1, the rest of the procedure was the same.
Distilled water was sufficiently absorbed by the temporary plugging agents prepared in examples 1 to 3 and comparative examples 1 to 3, and the distilled water was added to bentonite-based slurry (4% by mass of bentonite, 0.3% by mass of sodium carbonate, and the balance water) in an amount of 3%, and a sand bed plugging test was conducted under a pressure of 1MPa to examine the plugging ability of the temporary plugging agent to a 40-mesh sand bed at temperatures of 25 ℃, 80 ℃ and 180 ℃ and the results of the test are shown in table 1 below by an intrusion depth reaction.
TABLE 1
As can be seen from Table 1, the application has good blocking effect and can be kept stable under high temperature conditions.
The foregoing is merely illustrative and explanatory of the principles of the invention, as various modifications and additions may be made to the specific embodiments described, or similar thereto, by those skilled in the art, without departing from the principles of the invention or beyond the scope of the appended claims.
Claims (8)
1. The preparation method of the high-temperature-resistant temporary plugging agent for the oil field is characterized by comprising the following steps of:
Step A1, uniformly mixing tetramethyl cyclotetrasiloxane, 1-octene, chloroplatinic acid and DMF, introducing nitrogen for protection, and reacting to obtain a modified monomer;
A2, mixing octamethyl cyclotetrasiloxane, modified monomer, tetramethyl divinyl disiloxane, tetramethyl ammonium hydroxide and dimethyl sulfoxide, introducing nitrogen for protection, and reacting to obtain a modified crosslinking agent;
Step A3, uniformly mixing acrylamide, acrylic acid, 2-acrylamide-2-methylpropanesulfonic acid, castor oil and DMF, stirring, adding a modified crosslinking agent and a modified filler, stirring, adding dicumyl peroxide, and heating for reaction to obtain a high-temperature-resistant temporary plugging agent for oil fields;
the modified filler is prepared by the following steps:
Step B1, dispersing calcium carbonate in ethanol, stirring, adding KH550 and deionized water, reacting for 2-3h to obtain pretreated calcium carbonate, mixing the pretreated calcium carbonate, 3, 4-epoxy-1-butene and DMF, reacting, and modifying the calcium carbonate;
Step B2, uniformly mixing caprolactone, modified calcium carbonate, stannous octoate and DMF, introducing nitrogen for protection, reacting to obtain a precursor, uniformly mixing cellulose, chlorinated 1-butyl-3-methylimidazole and DMF, introducing nitrogen for protection, stirring, adding 2-bromo-2-methylpropanoyl bromide, and reacting to obtain pretreated cellulose;
And B3, dispersing the pretreated cellulose in DMF, introducing nitrogen for protection, stirring, adding thiourea, performing reaction, removing DMF, adding sodium hydroxide solution, performing reaction, adjusting pH to be acidic to obtain sulfhydryl cellulose, and mixing and reacting the sulfhydryl cellulose, a precursor, benzophenone and ethanol to obtain the modified filler.
2. The method for preparing the high-temperature-resistant temporary plugging agent for the oil field, which is disclosed in claim 1, wherein the molar ratio of the tetramethyl cyclotetrasiloxane to the 1-octene in the step A1 is 1:1.
3. The method for preparing the high-temperature-resistant temporary plugging agent for the oil field, which is disclosed in claim 1, wherein the molar ratio of the octamethyl cyclotetrasiloxane, the modified monomer, the tetramethyl divinyl disiloxane and the tetramethyl ammonium hydroxide in the step A2 is 1.6:0.8:1:2.
4. The preparation method of the high-temperature-resistant temporary plugging agent for the oil field, which is characterized in that the molar ratio of the acrylamide to the acrylic acid to the 2-acrylamide-2-methylpropanesulfonic acid to the castor oil in the step A3 is 15:1:4:2, the dosage of the modified cross-linking agent is 4 per mill of the sum of the masses of the acrylamide, the acrylic acid, the 2-acrylamide-2-methylpropanesulfonic acid and the castor oil, and the dosage of the modified filler is 5 per mill of the sum of the masses of the acrylamide, the acrylic acid, the 2-acrylamide-2-methylpropanesulfonic acid and the castor oil.
5. The method for preparing the high-temperature-resistant temporary plugging agent for the oil field, which is disclosed in claim 1, is characterized in that the dosage of KH550 in the step B1 is 1% of the mass of calcium carbonate, and the molar ratio of amino groups on the pretreated calcium carbonate to 3, 4-epoxy-1-butene is 1:2.
6. The preparation method of the high-temperature-resistant temporary plugging agent for the oil field, which is characterized in that the mass ratio of caprolactone to modified calcium carbonate to stannous octoate in the step B2 is 100:10:1, and the dosage ratio of cellulose to 1-butyl-3-methylimidazole chloride to 2-bromo-2-methylpropionamide is 1g:20g:12mL.
7. The preparation method of the high-temperature-resistant temporary plugging agent for the oil field, which is characterized in that the dosage ratio of the pretreated cellulose to the thiourea to the sodium hydroxide solution in the step B3 is 0.5 g/25 mmol/100 mL, and the mass ratio of the sulfhydryl cellulose to the precursor is 5:1.
8. A high-temperature-resistant temporary plugging agent for oil fields is characterized by being prepared by the preparation method according to any one of claims 1-7.
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| CN108059716A (en) * | 2018-01-09 | 2018-05-22 | 佳化化学（茂名）有限公司 | The polyurethane based on castor oil elastomer of its preparation of castor oil composite material and application |
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| CN109776728B (en) * | 2019-01-14 | 2021-02-12 | 中国石油大学(华东) | Temporary plugging agent for drilling fluid, preparation method of temporary plugging agent, water-based drilling fluid and application |
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