CN113429958B - Self-repairing fracturing fluid thickening agent and preparation method thereof - Google Patents
Self-repairing fracturing fluid thickening agent and preparation method thereof Download PDFInfo
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Abstract
A self-repairing fracturing fluid thickening agent and a preparation method thereof belong to the technical field of oilfield oil extraction additives. The gel fracturing fluid system based on hydrogen bond and Diels-Alder dynamic covalent bond, which is prepared by taking maleimide, furfural, N-dimethyl-1, 3-propane diamine, epichlorohydrin, acrylic acid, acrylamide and polyethylene glycol as main raw materials, can generate the capacity of instantaneous self-repairing when the gel is damaged in the fracturing process, thereby keeping the dynamic stability of the fracturing fluid system, preventing desanding in the fracturing process and ensuring the stability of pressure; meanwhile, the fracturing fluid system has the advantages of low friction resistance, easy gel breaking and easy flowback. The fracturing fluid system has excellent self-repairing capability and shows good stabilizing effect on the whole. The fracturing fluid thickening agent obtained by the invention has self-repairing capability and reliable preparation process, and can obviously improve the stability of the fracturing fluid.
Description
Technical Field
The invention belongs to the technical field of oil field production aids, and relates to a self-repairing fracturing fluid thickener and a preparation method thereof, in particular to a novel self-repairing gel fracturing fluid thickener based on hydrogen bonds and Diels-Alder dynamic covalent bonds and a preparation method thereof, and particularly relates to a novel self-repairing gel fracturing fluid thickener based on hydrogen bonds and Diels-Alder dynamic covalent bonds, which is obtained by taking maleimide, furfural, N-dimethyl-1, 3-propanediamine, epichlorohydrin, acrylic acid, acrylamide and polyethylene glycol as main raw materials, and a preparation method thereof.
Background
The fracturing is an important technical measure for increasing the yield of an oil-gas well and the injection of a water injection well, and plays an important role in improving the recovery ratio of crude oil, improving the water injection condition and the like. The purpose of fracturing construction is to achieve the maximum fracture conductivity within the limit range of design construction, and the quality of fracturing fluid is the most key factor of fracturing success or failure. In order to obtain a good hydraulic fracturing effect, the fracturing fluid is generally required to have the properties of strong sand suspending capacity, low friction resistance, good stability, easy flowback and the like.
The Chinese patent application with the publication number of CN103113875A discloses a water-based fracturing fluid thickening agent and a preparation method thereof. The thickener contains propylene glycolAcrylamide, 2-acrylamide-2 methyl-1-propanesulfonic acid, N-vinyl pyrrolidone, acrylic acid, a complexing agent, a chain transfer agent, a sodium hydroxide solution, an initiator and water. When the mass fraction of the prepared thickening agent in water-based fracturing fluid is 0.35%, the apparent viscosity is 140mPa & S, and the apparent viscosity is 170S-1And at 95 ℃, continuously shearing for 30min, wherein the viscosity retention rate is more than 60%.
The Chinese invention application with the publication number of CN105985765A discloses a fracturing fluid thickening agent, a preparation method thereof and a fracturing fluid. The fracturing fluid thickener comprises the following components: the high-performance composite material comprises acrylamide, unsaturated carboxylic acid, alkylphenol polyoxyethylene ether unsaturated acid ester, N-dimethyl-alkyl tertiary amine, halogenated cyclic ether, an initiator and water, wherein the sum of the mass percentages of the acrylamide, the unsaturated carboxylic acid, the alkylphenol polyoxyethylene ether unsaturated acid ester, the N, N-dimethyl-alkyl tertiary amine and the halogenated cyclic ether is 15-25%, and the mass percentage of the initiator is 0.04-0.09%.
The Chinese invention application with the publication number of CN106146730A discloses an acrylamide polymer thickener, a preparation method thereof and fracturing fluid, wherein the acrylamide polymer thickener comprises the following components: the thickening agent comprises the following components in percentage by mass: 20-45% of hydrophilic propenyl monomer, 4-6% of hydrophobic propenyl monomer, 1-2% of emulsifier, 0.2-0.5% of initiator, 0.5-1.8% of latent cross-linking agent and the balance of water, wherein the latent cross-linking agent accounts for 0.5-1.8% of the sum of the mass of the hydrophilic propenyl monomer and the mass of the hydrophobic propenyl monomer.
The jelly fracturing fluid formed by a series of polymers such as linear polysaccharide or polyacrylamide derivatives and the like used at present has the problem of poor stability, so that the sand removal is serious and the fracturing effect is poor in the construction process. Therefore, increasing the stability of the fracturing fluid is one of the important measures to improve the fracturing construction effect.
Disclosure of Invention
Through Diels-Alder reversible covalent bonds, the self-repairing hydrogel can spontaneously realize the repair of damaged parts after being damaged, and the mechanical property or function of the hydrogel is recovered, so that the hydrogel has excellent stability. The inventor finds that by utilizing the characteristic of the self-repairing hydrogel, the fracturing fluid with the self-repairing function can be prepared so as to solve the problem of instability of the fracturing fluid in the current fracturing construction.
The gel fracturing fluid system based on hydrogen bond and Diels-Alder dynamic covalent bond, which is prepared by taking maleimide, furfural, N-dimethyl-1, 3-propane diamine, epichlorohydrin, acrylic acid, acrylamide and polyethylene glycol as main raw materials, can generate the capacity of instantaneous self-repairing when the gel is damaged in the fracturing process, thereby keeping the dynamic stability of the fracturing fluid system, preventing desanding in the fracturing process and ensuring the stability of pressure; meanwhile, the fracturing fluid system has the advantages of low friction resistance, easy gel breaking and easy flowback. The fracturing fluid system has excellent self-repairing capability and shows good stabilizing effect.
In view of the technical requirement of fracturing construction on enhancing the stability of the fracturing fluid, the invention aims to provide a self-repairing fracturing fluid thickening agent and a preparation method thereof. Firstly, preparing N-epoxypropyl maleimide by taking maleimide and epoxy chloropropane as raw materials, and then reacting with acrylamide to prepare a monomer I; preparing N-furylmethyl-N, N-dimethyl-1, 3-propane diamine by taking furfural and N, N-dimethyl-1, 3-propane diamine as raw materials, reacting the product with epoxy chloropropane to prepare N-furylmethyl-N, N-dimethyl, N-epoxypropyl-1, 3-propane diamine, and reacting with acrylamide to prepare a monomer II; and then dissolving the two monomers, acrylic acid and acrylamide in proportion in distilled water, mixing with the distilled water solution dissolved with polyethylene glycol, and initiating polymerization under the action of an initiator to prepare the polymer with reversible hydrogen bonds and Diels-Alder dynamic covalent bonds. The polymer hydrogel has excellent self-repairing capability. The specific technical scheme is as follows.
The self-repairing fracturing fluid thickener is characterized by being a polymer with a side group containing carboxyl, amido, a maleimide skeleton and a furan skeleton.
Further, the monomers of the fracturing fluid thickening agent are respectively: preparing N-epoxypropyl maleimide from maleimide and epoxy chloropropane, and reacting with acrylamide to obtain a monomer I; preparing N-furylmethyl-N, N-dimethyl-1, 3-propane diamine by taking furfural and N, N-dimethyl-1, 3-propane diamine as raw materials, reacting the product with epoxy chloropropane to prepare N-furylmethyl-N, N-dimethyl, N-epoxypropyl-1, 3-propane diamine, and reacting with acrylamide to prepare a monomer II; acrylic acid and acrylamide.
Further, the monomer ratio of the fracturing fluid thickening agent is as follows: based on 100 parts of the monomer I, 90-110 parts of the monomer II, 180-220 parts of acrylic acid and 600-800 parts of acrylamide.
Parts are based on the amount of material (moles) unless otherwise indicated in the present invention.
Further, the preparation method of the self-repairing fracturing fluid thickener comprises the following steps:
(1) preparing N-epoxypropyl maleimide from maleimide and epoxy chloropropane, and reacting with acrylamide to prepare a monomer I;
(2) preparing N-furylmethyl-N, N-dimethyl-1, 3-propane diamine by taking furfural and N, N-dimethyl-1, 3-propane diamine as raw materials, reacting the product with epoxy chloropropane to prepare N-furylmethyl-N, N-dimethyl, N-epoxypropyl-1, 3-propane diamine, and reacting with acrylamide to prepare a monomer II;
(3) dissolving the monomer I, the monomer II, acrylic acid and acrylamide in distilled water according to a certain proportion, mixing with the distilled water solution dissolved with polyethylene glycol, introducing protective gas, and initiating polymerization reaction under the action of an initiator to prepare the polymer with reversible hydrogen bonds and Diels-Alder dynamic covalent bonds.
Further, the proportion of maleimide, epichlorohydrin and acrylamide in the step (1) is as follows: based on 100 parts of maleimide, 90-110 parts of epoxy chloropropane and 90-110 parts of acrylamide.
Further, the reaction in the step (1) is carried out under the protection of nitrogen; the reaction temperature of maleimide and epoxy chloropropane is 45-55 ℃, and the reaction time is 1-3 h; the reaction temperature of the N-epoxypropylmaleimide and the acrylamide is 60-70 ℃, and the reaction time is 2-4 h.
Further, in the step (2), the ratio of furfural, N-dimethyl-1, 3-propane diamine, epichlorohydrin and acrylamide is as follows: based on 100 parts of furfural, 90-110 parts of N, N-dimethyl-1, 3-propane diamine, 90-110 parts of epoxy chloropropane and 90-110 parts of acrylamide.
Further, the reaction in the step (2) is carried out under the protection of nitrogen; reacting furfural and N, N-dimethyl-1, 3-propane diamine at the temperature of 72-76 ℃ for 2-4 h, and cooling to 45-55 ℃; slowly dripping epoxy chloropropane, reacting at 45-55 ℃ for 1-3 h after dripping, and cooling to room temperature; and adding acrylamide into the solution, stirring for dissolving, heating to 60-70 ℃, and reacting for 2-4 hours.
Further, in the step (3), the ratio of the monomer I to the monomer II to the acrylic acid to the acrylamide is as follows: based on 100 parts of the monomer I, 90-110 parts of the monomer II, 180-220 parts of acrylic acid and 600-800 parts of acrylamide.
Further, in the step (3), the initiator is potassium persulfate.
Further, in the step (3), the protective gas is nitrogen, the polymerization reaction temperature is 65-75 ℃, and the polymerization reaction time is 2-4 hours.
The invention has the following beneficial technical effects: the fracturing fluid thickening agent obtained by the invention has self-repairing capability and reliable preparation process, and can obviously improve the stability of the fracturing fluid.
Detailed Description
The technical solution of the present invention is clearly and completely described below. It is to be understood that the described embodiments are merely exemplary of some, and not necessarily all, embodiments of the invention. All other embodiments, which can be obtained by a person skilled in the art without making creative efforts based on the embodiments of the present invention, belong to the protection scope of the present invention.
Example 1
A preparation method of a self-repairing fracturing fluid thickener comprises the following steps:
step (1): adding 0.02mol of maleimide and 20mL of absolute ethyl alcohol into a 100mL three-mouth reaction bottle, introducing nitrogen, stirring and dissolving, heating to 50 ℃, then slowly dropwise adding 0.02mol of epoxy chloropropane, requiring 1 hour, preserving heat at 50 ℃ after dropwise adding, reacting for 2 hours to obtain light yellow transparent liquid, cooling to room temperature, adding 0.02mol of acrylamide into the solution, stirring and dissolving, heating to 65 ℃, preserving heat, reacting for 3 hours to obtain yellow transparent liquid, distilling under reduced pressure, cooling to 5 ℃, precipitating light yellow crystals, filtering, drying, and preserving at room temperature for later use.
Step (2): adding 0.02mol of furfural, 1.0g of p-toluenesulfonic acid and 20mL of a methanol-water mixed solvent (the mass ratio is 1: 1) into a 100mL three-mouth reaction bottle, introducing nitrogen, stirring for dissolving, then adding 0.02mol of N, N-dimethyl-1, 3-propanediamine, heating to 74 ℃, reacting for 3 hours to obtain yellow liquid, cooling to 50 ℃, then slowly dropwise adding 0.02mol of epoxy chloropropane for 1 hour, keeping the temperature at 50 ℃ for reacting for 2 hours after dropwise adding to obtain yellow liquid, cooling to room temperature, adding 0.02mol of acrylamide into the solution, adding 10mL of anhydrous methanol, stirring for dissolving, heating to 65 ℃, keeping the temperature for reacting for 3 hours to obtain yellow transparent liquid, distilling under reduced pressure, cooling to 5 ℃, precipitating yellow crystals, filtering, drying, and storing at room temperature for later use.
And (3): adding the products generated in the steps (1) and (2) into a 250mL reaction bottle, adding 0.04mol of acrylic acid, 0.14mol of acrylamide and 50mL of distilled water, and stirring for dissolving; dissolving 5.0 g of polyethylene glycol-6000 in 30mL of distilled water, then uniformly mixing the two solutions, adding 0.003g of potassium persulfate, stirring to dissolve, introducing nitrogen for 20 minutes, heating to 70 ℃ to initiate polymerization, requiring 3 hours, and cooling to room temperature to obtain yellow colloid.
Example 2
The yellow colloid prepared in step (3) of example 1 was accurately weighed, stirred and dissolved in clear water to prepare sample solutions having drug concentrations of 0.1%, 0.2% and 0.3%, respectively. Measuring the viscosities of the solutions with various concentrations at 30 ℃, 60 ℃ and 90 ℃ by using a BROOKFILD DV-III + type rheometer; the results are shown in Table 1.
TABLE 1 viscosity (mPa. s) of aqueous solutions of samples at different concentrations and temperatures
As can be seen from table 1, at the three concentrations of 0.1%, 0.2% and 0.3%, the viscosity of the solution increases with increasing concentration of the sample, the viscosity of the 0.3% aqueous solution being greater than 2 times the viscosity of the 0..1% aqueous solution; in addition, the solution viscosity slightly decreases with increasing temperature for the same sample concentration.
Example 3
The yellow colloid prepared in step (3) of example 1 was accurately weighed, stirred and dissolved in clear water to prepare sample solutions having drug concentrations of 0.1%, 0.2% and 0.3%, respectively. Each of the above solutions was sheared using an RV20 rheometer at a shear rate of 170s-1The shearing time is 10 minutes, and then the viscosity of each solution after shearing is measured at three temperatures of 30 ℃, 60 ℃ and 90 ℃ for different times, and the results are shown in tables 2 to 4.
Table 230 ℃ viscosity of the sample solution after shearing for different times (mpa.s)
Table viscosity (mpa.s) of the sample solutions at 360 ℃ after shearing for different times
TABLE viscosity (mPa.s) of the sample solutions at 490 ℃ after shearing for different times
As can be seen from tables 2 to 4, the shear rate is 170s at three temperatures of 30 ℃, 60 ℃ and 90 ℃-1Shear time of 10 minutes, three concentrations of solution at 2 minutesThe viscosity substantially returns to that before shearing after a while. The solution has better self-repairing capability.
Example 4
The yellow transparent colloid prepared in step (3) of example 1 was accurately weighed, cut into small pieces, stirred, and dissolved in clear water to prepare solutions having concentrations of 0.1%, 0.2%, and 0.3%, respectively. Under the three temperature conditions of 30 ℃, 60 ℃ and 90 ℃, the ammonium persulfate microcapsules are used as gel breakers, the addition is 0.05 percent of the solution, gel breaking is carried out on various solutions, and the viscosity of each solution is measured after 30 minutes, and the results are shown in table 5.
TABLE 5 viscosity (mPa.s) of each solution after 30 minutes of gel breaking at different concentrations and temperatures
Comparing the data in table 5 and table 1, it can be seen that the viscosity of the solution is greatly reduced and is lower than 5 mpa.s after the solution is oxidized and broken by ammonium persulfate, which indicates that the sample solution has better broken capacity.
Although some embodiments of the present invention have been shown and described above, it is understood that the above embodiments are exemplary and should not be construed as limiting the present invention, and those skilled in the art can make variations, modifications, substitutions and alterations within the scope of the present invention without departing from the principle and spirit of the invention. The scope of the invention is defined by the claims and their equivalents.
Claims (9)
1. The self-repairing fracturing fluid thickener is characterized by being a polymer with a side group containing carboxyl, amido, maleimide skeleton and furan skeleton, and the monomers of the fracturing fluid thickener are as follows: preparing N-epoxypropyl maleimide from maleimide and epoxy chloropropane, and reacting with acrylamide to obtain monomer
(ii) a Preparing N-furylmethyl-N, N-dimethyl-1, 3-propane diamine by taking furfural and N, N-dimethyl-1, 3-propane diamine as raw materials, reacting the product with epoxy chloropropane to prepare N-furylmethyl-N, N-dimethyl, N-epoxypropyl-1, 3-propane diamine, and reacting with acrylamide to prepare the monomer
(ii) a Acrylic acid and acrylamide.
2. The fracturing fluid thickener of claim 1, wherein the monomer ratio of the fracturing fluid thickener is: in the form of a single body
Based on 100 parts of monomer
90-110 parts of acrylic acid, 180-220 parts of acrylic acid and 600-800 parts of acrylamide.
3. The method for preparing the fracturing fluid thickener according to claim 1 or 2, comprising the steps of:
(1) preparing N-epoxypropyl maleimide from maleimide and epoxy chloropropane, and reacting with acrylamide to obtain monomer
；
(2) Preparing N-furylmethyl-N, N-dimethyl-1, 3-propane diamine by taking furfural and N, N-dimethyl-1, 3-propane diamine as raw materials, reacting the product with epoxy chloropropane to prepare N-furylmethyl-N, N-dimethyl, N-epoxy propyl-1, 3-propane diamine, and reacting with acrylamide to prepare a monomer
；
(3) Mixing the above monomers
Monomer, monomer
Acrylic acid and acrylamide are dissolved in distilled water according to a certain proportion, then are mixed with distilled water solution in which polyethylene glycol is dissolved, protective gas is introduced, and then polymerization reaction is initiated under the action of an initiator, so as to prepare the polymer with reversible hydrogen bonds and Diels-Alder dynamic covalent bonds.
4. The process according to claim 3, wherein the proportions of maleimide, epichlorohydrin and acrylamide in step (1) are as follows: based on 100 parts of maleimide, 90-110 parts of epoxy chloropropane and 90-110 parts of acrylamide.
5. The preparation method according to claim 3, wherein the reaction in step (1) is carried out under nitrogen protection; the reaction temperature of maleimide and epoxy chloropropane is 45-55 ℃, and the reaction time is 1-3 h; the reaction temperature of the N-epoxypropylmaleimide and the acrylamide is 60-70 ℃, and the reaction time is 2-4 h.
6. The preparation method according to claim 3, wherein the ratio of furfural, N-dimethyl-1, 3-propanediamine, epichlorohydrin and acrylamide in step (2) is as follows: based on 100 parts of furfural, 90-110 parts of N, N-dimethyl-1, 3-propane diamine, 90-110 parts of epoxy chloropropane and 90-110 parts of acrylamide.
7. The preparation method according to claim 3, wherein the reaction in step (2) is carried out under nitrogen protection; reacting furfural and N, N-dimethyl-1, 3-propane diamine at the temperature of 72-76 ℃ for 2-4 h, and cooling to 45-55 ℃; slowly dripping epoxy chloropropane, reacting at 45-55 ℃ for 1-3 h after dripping, and cooling to room temperature; and adding acrylamide into the solution, stirring for dissolving, heating to 60-70 ℃, and reacting for 2-4 hours.
8. The production method according to claim 3, wherein the monomer in the step (3)
Monomer (b)
The ratio of acrylic acid to acrylamide is: by a single body
Based on 100 parts of monomer
90-110 parts of acrylic acid, 180-220 parts of acrylic acid and 600-800 parts of acrylamide.
9. The production method according to claim 3, wherein the initiator in the step (3) is potassium persulfate; in the step (3), the protective gas is nitrogen, the polymerization reaction temperature is 65-75 ℃, and the polymerization reaction time is 2-4 h.
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| CN105985765B (en) * | 2015-02-16 | 2018-10-16 | 中国石油天然气股份有限公司 | Fracturing fluid thickening agent, preparation method thereof and fracturing fluid |
| CN107973886A (en) * | 2016-10-24 | 2018-05-01 | 中国林业科学研究院林产化学工业研究所 | A kind of preparation of thermal reversion self-healing polymers material and restorative procedure |
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