CN115261008A - Preparation method of fracturing fluid with double-slow crosslinking system - Google Patents
Preparation method of fracturing fluid with double-slow crosslinking system Download PDFInfo
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Abstract
The invention discloses a preparation method of fracturing fluid with a crosslinking system with double slow release performance, which is implemented according to the following steps: step 1, adding methanol into a three-neck flask, adding ferroceneboronic acid, uniformly mixing, dropwise adding a ligand, and heating to a certain temperature to react to obtain a cross-linking agent; step 2, crosslinking the crosslinking agent prepared in the step 1 with a thickening agent to obtain fracturing fluid of a slow-release crosslinking system; and 3, adding peroxyacetic acid into the fracturing liquid system of the slow-release crosslinking system prepared in the step 2 to obtain the fracturing liquid of a double-slow system. After the fracturing fluid is oxidized, the iron in the ferrocene presents a ferric ion state and is slowly broken with the oxidant, so that the phenomenon of too early reduction of the viscosity of the fracturing fluid is avoided, and the problems of poor slow release performance and poor high temperature resistance of the conventional fracturing fluid are solved.
Description
Technical Field
The invention belongs to the technical field of oil field fracturing, and relates to a preparation method of a fracturing fluid with a double-slow-performance crosslinking system.
Background
With the development of the petroleum industry, the exploitation of deep well high temperature oil reservoirs is more and more important, and the conventional crosslinking system cannot meet the requirement of the exploitation of the high temperature oil reservoirs. The conventional crosslinking system has two defects, namely, the high crosslinking speed can cause the flowing resistance of the fracturing fluid in a pipeline to be increased and too much power to be consumed; and secondly, the fracturing fluid is continuously sheared in the deep well, and the performance of the fracturing fluid is difficult to maintain.
The development of the delayed gel breaking technology mainly focuses on delaying gel breakers, such as degradable solid particle high polymer delayed gel breakers and packer gel breakers. The degradable solid particle delayed gel breaker is a concentrated product of organic acid, the polymer can be hydrated and degraded at the temperature of above 66 ℃ to generate acid, and the acid acts on jelly to break the gel by hydration, but the delayed gel breaker is greatly influenced by temperature. The packing gel breaker is a granular gel breaker prepared by wrapping packing materials outside the granular gel breaker by utilizing a surface coating technology. The packing material can be water-soluble polymer, degradable polymer or polymer which is insoluble in water, acid and alkali and high temperature. The gel breaker can be an enzyme (such as aspergillus flavus enzyme and aspergillus niger) or an oxide gel breaker (such as persulfate) and the like. The gel breaker has the function of delaying gel breaking due to the coating treatment on the surface of the gel breaker. But the gel breaking delaying effect is closely related to the characteristics of the packing material, environmental factors (such as temperature) and the like. The delayed crosslinking agent plays a role in delaying crosslinking, so that the fracturing fluid cannot be crosslinked when flowing in a ground pipeline, and the fracturing fluid with the required viscosity is gradually formed in a target layer. The method is beneficial to construction pumping and can keep the good performance of the fracturing fluid. In the aspect of delayed crosslinking technology, the delayed crosslinking technology is mainly realized by the following two aspects, namely, the delayed crosslinking technology is realized by adjusting the pH value of a base fluid. For example, boron crosslinked guar gum and its derivatives are delayed crosslinking systems, in which a boron crosslinking agent and a gelling agent are first formulated into an acidic solution, and since the boron jelly is crosslinked under alkaline conditions to form the boron jelly, no crosslinking occurs. Then adding a hydrophobic alkaline slurry into the base liquid and dispersing the slurry in the base liquid, wherein the pH value of the system is changed, so that the system has the effect of delaying crosslinking, but the requirement of the technology on the pH is too severe. On the other hand, the slow release technology is realized through the action of the ligand and the crosslinking center preferentially. By introducing the organic ligand into the cross-linking agent, the ligand can preferentially react with the cross-linking central ions, and the reaction speed between the cross-linking central ions and the gelling agent molecules is inhibited, so that the system shows a good slow cross-linking effect. However, at higher temperatures, the slow crosslinking action is not significant. After fracturing construction is finished, a gel breaker is usually needed to enable fracturing fluid to be rapidly and completely hydrated and broken and smoothly flow back, but the conventional gel breaker starts to act with the fracturing fluid to break gel after being added from a wellhead pipeline, so that the performance of the fracturing fluid is deteriorated.
Disclosure of Invention
The invention aims to provide a preparation method of a fracturing fluid with a double-slow-release crosslinking system, which solves the problem of poor slow-release performance and high-temperature resistance of the conventional fracturing fluid.
The technical scheme adopted by the invention is that the preparation method of the fracturing fluid with a double-slow crosslinking system is implemented according to the following steps:
step 1, adding methanol and ferrocene modified boric acid into a three-neck flask with a stirring and condensing reflux device, uniformly mixing, dropwise adding a ligand, and heating to a certain temperature to react to prepare a cross-linking agent;
step 2, crosslinking the crosslinking agent prepared in the step 1 with a thickening agent to obtain fracturing fluid of a slow-release crosslinking system;
and 3, adding an oxidant into the fracturing liquid system of the slow-release crosslinking system prepared in the step 2 to obtain the fracturing liquid of the double-slow system.
The present invention is also characterized in that,
in the step 1, methanol is used as a solvent, ferrocene modified boric acid and a ligand are used as reaction liquid, and the mass fraction of the reaction liquid is 45-55%; the mass fraction of the ferrocene modified boric acid accounts for 60-80% of the reaction liquid, and the mass fraction of the ligand accounts for 20-40% of the reaction liquid.
The reaction temperature in the step 1 is 50-60 ℃; the reaction time is 4-6 h.
In the step 1, the ferrocene modified boric acid adopts any one of ferrocene boric acid and 1, 1-ferrocene diboronic acid.
In the step 1, citric acid and triethanolamine are adopted as ligands, and the ratio of the citric acid to the triethanolamine is 1.
In the step 2, water is used as a solvent, the concentration of the thickening agent is 0.6-1%, and the addition amount of the cross-linking agent is 0.4-1% of the mass of the thickening agent solution.
And 3, the mass fraction of the oxidant is 0.4-0.6% of the slow-release fracturing fluid system.
The oxidant is any one of peroxyacetic acid, hydrogen peroxide and potassium permanganate.
The thickening agent adopts any one of guar gum, hydroxypropyl guar gum or guar gum derivatives.
The beneficial effects of the invention are: according to the preparation method of the fracturing fluid with the double-slow-release crosslinking system, the crosslinking agent adopts ferrocene modified boric acid to replace boric acid or borax in the original crosslinking system, the ferrocene modified boric acid combines the crosslinking center ion ligands through covalent bonds, so that the speed of releasing the crosslinking center boron ions is rapidly slowed down, and the crosslinking center boron ions can be completely released under the high-temperature condition, so that the fracturing fluid has good slow release performance and temperature resistance, and the slow release time is over 10 min. The invention discloses a fracturing fluid, which is prepared by adopting a ferrocene and peracetic acid redox breaking technology, wherein iron in oxidized ferrocene is in a ferric ion state, and the ferric ion and peracetic acid can realize slow gel breaking, so that the phenomenon of premature reduction of the viscosity of the fracturing fluid is avoided, and the problems of poor slow release performance and high temperature resistance of the existing fracturing fluid are solved.
Drawings
FIG. 1 is a schematic diagram illustrating the synthetic principle of the cross-linking agent of the method for preparing the fracturing fluid with a crosslinking system with double buffering capacity;
FIG. 2 is a schematic diagram of the crosslinking operation of the double retarded system of the method for preparing the fracturing fluid with the double retarded crosslinking system according to the present invention;
FIG. 3 is a gel breaking diagram of a double retarded system of the fracturing fluid preparation method with a double retarded crosslinking system according to the present invention;
FIG. 4 is a viscosity-temperature diagram of a dual retarded system fracturing fluid prepared in example 3 of this invention.
Detailed Description
The invention is described in detail below with reference to the following figures and embodiments:
the preparation method of the fracturing fluid with the crosslinking system with double slow release performance is implemented according to the following steps:
step 1, adding methanol and ferrocene modified boric acid into a three-neck flask with a stirring and condensing reflux device, uniformly mixing, then dropwise adding a ligand, heating to a certain temperature, and reacting to prepare a cross-linking agent, wherein the principle is shown in figure 1;
in the step 1, methanol is used as a solvent, ferrocene modified boric acid and a ligand are used as reaction liquid, and the mass fraction of the reaction liquid is 45-55%; the mass fraction of the ferrocene modified boric acid accounts for 60-80% of the reaction liquid, and the mass fraction of the ligand accounts for 20-40% of the reaction liquid; the reaction temperature is 50-60 ℃; the reaction time is 4-6 h.
The ferrocene modified boric acid adopts any one of ferrocene boric acid and 1, 1-ferrocene diboronic acid.
The ligand adopts citric acid and triethanolamine, and the ratio of the citric acid to the triethanolamine is 1.
Step 2, crosslinking the crosslinking agent prepared in the step 1 with a thickening agent, wherein the principle is shown in figure 2; obtaining fracturing fluid of a slow-release crosslinking system; in the step 2, water is used as a solvent, and the concentration of the thickening agent is 0.6-1%. The addition amount of the cross-linking agent is 0.4-1% of the mass of the thickening agent solution.
Step 3, adding an oxidant into the fracturing liquid system of the slow-release crosslinking system prepared in the step 2, wherein the principle is shown in figure 3; obtaining the fracturing fluid of a double-slow system.
The mass fraction of the oxidant is 0.4-0.6% of the slow-release fracturing fluid system.
The oxidant is any one of peroxyacetic acid, hydrogen peroxide and potassium permanganate;
the thickening agent adopts any one of guar gum, hydroxypropyl guar gum or guar gum derivatives.
According to the preparation method of the crosslinking system fracturing fluid with double slow release performance, the prepared crosslinking agent adopts ferrocene modified boric acid to replace boric acid or borax in the original crosslinking system, the speed of releasing boron ions in a crosslinking center by the ferrocene boric acid is rapidly reduced, and the boron ions in the crosslinking center can be completely released under the high-temperature condition, so that the crosslinking system fracturing fluid has good slow release performance and temperature resistance, and the slow release time is over 10 min. The gel breaking process of the fracturing fluid adopts a ferrocene and peracetic acid redox breaking technology, iron in the oxidized ferrocene is in a ferric ion state, and slow gel breaking can be realized with peracetic acid, so that the performance deterioration of the fracturing fluid is avoided.
Example 1
The preparation method of the crosslinking system fracturing fluid with double buffering performance provided by the embodiment is implemented according to the following steps:
adding 100g of methanol into a three-neck flask with stirring and condensation reflux, adding 30g of ferroceneboronic acid, uniformly mixing, dropwise adding 10g of citric acid and 10g of triethanolamine, heating to 50 ℃, and reacting for 4 hours to obtain the cross-linking agent. 0.6g of cross-linking agent and 100g of 0.6% guanidine gum thickening agent are taken for cross-linking, and 0.5g of peroxyacetic acid is added into the fracturing fluid system of the slow-release cross-linking system to obtain the fracturing fluid of the double-slow system.
Example 2
The preparation method of the crosslinking system fracturing fluid with double buffering performance provided by the embodiment is implemented according to the following steps:
adding 100g of methanol into a three-neck flask with stirring and condensation reflux, adding 40g of 1, 1-ferrocene diboronic acid, dropwise adding 5g of citric acid and triethanolamine after uniformly mixing, and heating to 60 ℃ to react for 6 hours to obtain the cross-linking agent. And (3) crosslinking 0.8g of crosslinking agent and 100g of hydroxypropyl guar gum thickening agent with the concentration of 0.8%, and adding 0.6g of hydrogen peroxide into the fracturing fluid system of the slow-release crosslinking system to obtain the fracturing fluid of a double-slow system.
Example 3
The preparation method of the crosslinking system fracturing fluid with double buffering performance provided by the embodiment is implemented according to the following steps:
100g of methanol is added into a three-neck flask with stirring and condensation reflux, 35g of ferroceneboronic acid is added, 7.5g of citric acid and 7.5g of triethanolamine are respectively added dropwise after uniform mixing, and the temperature is raised to 55 ℃ for reaction for 6 hours to obtain the cross-linking agent. 0.8g of cross-linking agent and 100g of guanidine gum thickening agent with the concentration of 0.6% are taken for cross-linking, 0.5g of peroxyacetic acid is added into the fracturing fluid system of the slow-release cross-linking system to obtain the fracturing fluid of a double-slow system, and in order to represent the viscosity of the prepared fracturing fluid under the condition of temperature change, the fracturing fluid prepared in the example 3 is subjected to shear rate of 170s-1The temperature resistance test was carried out under the conditions (1), and the results are shown in FIG. 4, from FIG. 4, it can be seen that the temperature resistance test was carried out at 170s-1Under the shear rate of (2), the viscosity of the energized fracturing fluid can still be kept at about 50mPa & s when the temperature is increased to 180 ℃, and the energized fracturing fluid can resist the temperature of 180 ℃ and has good temperature resistance.
Because the cross-linking agent has the effect of delaying cross-linking and the effect of delaying gel breaking when the fracturing fluid breaks the gel, in order to represent the slow release performance of the cross-linking agent, the gel of the fracturing fluid and the gel breaking are tested, and meanwhile, the existing fracturing fluid technology is used for comparison. The results are shown in Table 1.
Table 1 prepared viscous slow release performance data for the dual slow system fracturing fluids
The slow release performance data show in table 1 that the synthesized slow release system has delayed crosslinking time of more than 10min, increased gel breaking delay of 30min and excellent slow release effect.
Example 4
The preparation method of the crosslinking system fracturing fluid with double buffering performance provided by the embodiment is implemented according to the following steps:
100g of methanol and 38g of ferroceneboronic acid are added into a three-neck flask with stirring and condensation reflux, 6g of citric acid and 6g of triethanolamine are dropwise added after uniform mixing, and the temperature is raised to 60 ℃ for reaction for 5 hours to obtain the cross-linking agent. And (3) crosslinking 0.7g of crosslinking agent and 100g of 0.7% guanidine gum thickening agent, and adding 0.8g of peroxyacetic acid into the fracturing liquid system of the slow-release crosslinking system to obtain the fracturing liquid of the double-slow system.
Example 5
The preparation method of the crosslinking system fracturing fluid with double buffering performance provided by the embodiment is implemented according to the following steps:
100g of methanol is added into a three-neck flask with stirring and condensation reflux, 36g of ferroceneboronic acid is added, 7g of citric acid and 7g of triethanolamine are added dropwise after uniform mixing, and the temperature is raised to 55 ℃ for reaction for 5 hours to obtain the cross-linking agent. And (3) crosslinking 0.8g of crosslinking agent and 100g of 0.8% guanidine gum thickening agent, and adding 1g of potassium permanganate into the fracturing liquid system of the slow-release crosslinking system to obtain the fracturing liquid of the double-slow system.
According to the preparation method of the fracturing fluid with the double-slow-release crosslinking system, the prepared crosslinking agent adopts ferroceneboronic acid to replace boric acid or borax in the original crosslinking system, the ferroceneboronic acid combines a crosslinking center ion ligand through a covalent bond, so that the speed of releasing the crosslinking center boron ions is rapidly reduced, and the crosslinking center boron ions can be completely released under the high-temperature condition, so that the fracturing fluid has good slow release performance and temperature resistance, and the slow release time is over 10 min. Meanwhile, the gel breaking process of the fracturing fluid adopts a ferrocene and peracetic acid redox breaking technology, and iron in the oxidized ferrocene is in a ferric ion state and can realize slow gel breaking with peracetic acid. Ferrocene boric acid is introduced into the system to play a role in slowly releasing crosslinking central ions; after the crosslinking is finished, peroxyacetic acid and ferric ions are subjected to oxidation-reduction reaction to realize gel breaking. During preparation, in order to ensure slow release, excessive ferrocene boric acid reacts with citric acid and triethanolamine to form a compound through coordination and complexation, and the compound is slowly released when meeting a thickening agent.
Claims (9)
1. The preparation method of the fracturing fluid with the double-slow crosslinking system is characterized by comprising the following steps:
step 1, adding methanol and ferrocene modified boric acid into a three-neck flask with a stirring and condensing reflux device, uniformly mixing, dropwise adding a ligand, and heating to a certain temperature to react to prepare a cross-linking agent;
step 2, crosslinking the crosslinking agent prepared in the step 1 with a thickening agent to obtain fracturing fluid of a slow-release crosslinking system;
and 3, adding an oxidant into the fracturing liquid system of the slow-release crosslinking system prepared in the step 2 to obtain the fracturing liquid of the double-slow system.
2. The preparation method of the fracturing fluid with the crosslinking system having the double buffering performance as claimed in claim 1, wherein in the step 1, methanol is used as a solvent, ferrocene modified boric acid and a ligand are used as a reaction solution, and the mass fraction of the reaction solution is 45-55%; the mass fraction of the ferrocene modified boric acid accounts for 60-80% of the reaction liquid, and the mass fraction of the ligand accounts for 20-40% of the reaction liquid.
3. The preparation method of the fracturing fluid with the double-slow crosslinking system according to claim 2, wherein the reaction temperature in the step 1 is 50-60 ℃; the reaction time is 4-6 h.
4. The preparation method of the fracturing fluid with the double-buffering-performance crosslinking system according to claim 2, wherein in the step 1, the ferrocene modified boric acid is any one of ferrocene boric acid and 1, 1-ferrocene diboronic acid.
5. The method for preparing the fracturing fluid with the crosslinking system with the double slowing performance as claimed in claim 1, wherein the ligand in the step 1 is citric acid and triethanolamine, and the ratio of the citric acid to the triethanolamine is 1.
6. The preparation method of the fracturing fluid with the double-buffering crosslinking system according to claim 1, wherein in the step 2, water is used as a solvent, the concentration of the thickening agent is 0.6-1%, and the addition amount of the crosslinking agent is 0.4-1% of the mass of the thickening agent solution.
7. The preparation method of the fracturing fluid with the double-slow-release crosslinking system according to claim 1, wherein the mass fraction of the oxidizing agent in the step 3 is 0.4-0.6% of the slow-release fracturing fluid system.
8. The preparation method of the fracturing fluid with the double-buffering crosslinking system according to claim 1, wherein the oxidant is any one of peroxyacetic acid, hydrogen peroxide and potassium permanganate.
9. The method for preparing the fracturing fluid with the crosslinking system with double buffering performance of claim 1, wherein the thickening agent is guanidine gum, hydroxypropyl guanidine gum or any one of guanidine gum derivatives.
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