CN109609113B - Temperature-resistant composite clean fracturing fluid and preparation method thereof - Google Patents
Temperature-resistant composite clean fracturing fluid and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a temperature-resistant composite clean fracturing fluid and a preparation method thereof, wherein the temperature-resistant composite clean fracturing fluid comprises the following components in percentage by mass: 1-2% of a surfactant; 1-2% of a counter ion auxiliary agent; 1-2% of nano particles; the balance being water. The preparation method comprises the following steps: the preparation method comprises the steps of firstly carrying out esterification reaction on common hydrophilic nano silicon dioxide and an anhydride organic matter to obtain anhydride modified surface carboxylated nano particles, then preparing nano fluid by using the modified nano particles, sequentially adding a temperature-resistant surfactant and a counter ion assistant, uniformly mixing, standing at a constant temperature, and standing to obtain the temperature-resistant composite clean fracturing fluid. The preparation method of the temperature-resistant composite clean fracturing fluid is simple and low in cost, and the nanometer silicon dioxide particles modified by the anhydride have double mechanism effects in the clean fracturing fluid to further strengthen the gel forming structure of the long-chain surfactant, so that the viscoelasticity and the temperature resistance of the clean fracturing fluid are improved, and the application of the clean fracturing fluid in a complex reservoir is widened.
Description
Technical Field
The invention belongs to the technical field of functional nano materials and oil extraction chemistry in oil and gas field development, and particularly relates to a temperature-resistant composite clean fracturing fluid and a preparation method thereof.
Background
With the rapid development of national economy, petroleum is used as an efficient and wide energy source, and the demand for the petroleum is continuously increased. With the continuous progress of oil and gas exploration and development, the reserves of easy-to-recover reservoirs are continuously reduced, so the development aiming at low-permeability hydrocarbon reservoirs is in a technical reserve stage at present. The hypotonic hydrocarbon reservoir in China contains rich oil and gas reserves, but the effective production cannot be realized depending on the self energy due to the lower natural productivity, so the recovery ratio must be improved by a fracturing method, wherein the fracturing fluid is one of important influencing factors of a fracturing process and is called fracturing blood. The common types of fracturing fluids in oil fields at present comprise water-based fracturing fluids, oil-based fracturing fluids, foam fracturing fluids and the like. With the current green chemistry, the clean fracturing fluid prepared by the viscoelastic surfactant has the characteristics of good viscoelasticity, low damage to stratum, no residue and the like, and becomes a research focus in recent years. However, the conventional clean fracturing fluid has the problems of insufficient stability, poor temperature resistance and the like in practical application.
In order to overcome the above problems, researchers have sought novel viscoelastic surfactants to obtain fracturing fluid systems with higher strength and better temperature resistance, and CN107445857A discloses a fracturing fluid system with CO2The preparation method of long-chain alkyl acid amide propyl dimethylamine with response performance prepares a long-chain structure and CO pair through synthetic reaction2The responsive surfactant has longer tail chain and better temperature resistance, and CO is introduced2Then gel with certain strength can be formed. However, the gel prepared by the invention can not exist stably for a long time when CO exists2After the gel is consumed, the viscosity of the gel is gradually reduced along with the time, and the later requirement of the fracturing process cannot be met. The invention patent CN 103320114B discloses a multi-association polymer clean fracturing fluid thickener, and the evaluation indexes are as follows: the viscosity of 0.3% water solution is more than or equal to 30 mPa.s at 20 ℃; the viscosity of the solution after gel breaking is less than or equal to 5mPa & s; the static sand suspending time is more than or equal to 10 min. However, the synthesis process of the associated long-carbon chain alkyl acrylamide polymer provided by the invention is complex, the cost of related chemicals is high, and the polymer monomer is easy to remain in the stratum and cannot be degraded.
The performance of the clean fracturing fluid is further enhanced by utilizing a nano material, which also becomes one of the current research hotspots, and CN 107033868A discloses a nano material enhanced clean fracturing fluid and a preparation method thereof, wherein a novel composite clean fracturing fluid system is obtained by compounding a quaternary ammonium salt cationic surfactant and nano silicon dioxide, the consistency and viscoelasticity of the fracturing fluid can be further improved, and the function of improving the performance of the fracturing fluid of the nano silicon dioxide is verified. The invention patent CN 104927799A discloses a carbon nano tube composite thickening agent and a preparation method thereof, wherein the thickening agent comprises the following components in parts by weight: 1-5% of viscoelastic surfactant, 0.05-0.4% of modified carbon nanotube particles, 0-8% of counter ion salt, 0-3% of auxiliary agent and the balance of water to 100%, wherein the components are mixed and stirred uniformly according to the proportion to prepare the carbon nanotube composite thickening agent.
Although the current situation and the defects of the clean fracturing fluid can be improved by the current research aiming at the clean fracturing fluid, the defects of low application range, high cost, single action mechanism of the nano material, insufficient temperature resistance, incapability of large-scale application and the like still exist.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides the temperature-resistant composite clean fracturing fluid which is simple in preparation method and low in cost, and the colloid forming structure of the long-chain surfactant is further strengthened by utilizing the novel anhydride modified nano silicon dioxide particles, so that the viscoelasticity and the temperature resistance of the clean fracturing fluid are improved, and the application of the clean fracturing fluid in a complex reservoir stratum is widened.
In order to achieve the purpose, the technical scheme of the invention is a temperature-resistant composite clean fracturing fluid which comprises the following components in percentage by mass:
1-2% of a surfactant; 1-2% of a counter ion auxiliary agent; 1-2% of nano particles; the balance being water.
Further, the surfactant is a pH sensitive type long-chain alkyl acid amide propyl dimethylamine compound; the surfactant is one of behenamidopropyl dimethylamine, stearic acid amidopropyl dimethylamine, palmitic acid amidopropyl dimethylamine or erucic acid amidopropyl dimethylamine.
Further, the counter ion auxiliary agent is one of sodium salicylate, sodium nitrate, sodium maleate, sodium dodecyl sulfate, sodium dodecyl benzene sulfonate or sodium p-toluenesulfonate.
Further, the nanoparticles are modified nanoparticles; the modified nano-particle is hydrophilic nano-silica particle which is subjected to surface modification by using an anhydride organic matter.
Preferably, the acid anhydride organic substance is one of succinic anhydride, glutaric anhydride, maleic anhydride, trimellitic anhydride, and phthalic anhydride.
Further, the preparation method of the modified nano-particles comprises the following steps:
A. dispersing common hydrophilic nano silicon dioxide in an organic solvent by using an ultrasonic cleaner, then adding an anhydride organic substance, and magnetically stirring for 15 hours at room temperature at the rotating speed of 600-;
B. and C, placing the anhydride modified nano-particle reaction liquid obtained in the step A into a high-speed centrifuge for high-speed centrifugation at 9000 revolutions for 30 minutes, collecting a centrifugal product, washing for 3 times by using ethanol to remove the anhydride organic matters which are not completely reacted, after the ethanol washing is finished, carrying out vacuum drying to remove the residual organic solvent and ethanol, and grinding the dried solid to obtain the anhydride modified nano-silica particles.
Preferably, in the step A, the particle diameter of the common hydrophilic nano-silica is 15-25nm, and the specific surface area is 240-380m2The surface group is hydroxyl group, and the mass percentage in the reaction stock solution is 1-2%.
Preferably, in step a, the organic solvent is any one of toluene, cyclohexane or N, N-dimethylamide.
Preferably, in the step A, the mass ratio of the acid anhydride organic matter to the common hydrophilic nano silicon dioxide particles is 3-4: 3.
Further, the invention also provides a preparation method of the temperature-resistant composite clean fracturing fluid, which comprises the following steps:
(1) adding the nano particles into water, mechanically stirring for 30 minutes under the condition of the rotation speed of 500 plus 600 revolutions per minute until the solution is uniform, then placing the solution into an ultrasonic cleaner, and ultrasonically dispersing for 3 hours at 50 ℃ until the solution is clear and transparent to obtain a nano fluid;
(2) and (2) taking the nanofluid prepared in the step (1) as a base fluid, sequentially adding a surfactant and a counter-ion auxiliary agent, uniformly mixing, and then placing into a 50 ℃ water bath kettle to stably stand for 2-2.5 hours to obtain the temperature-resistant composite clean fracturing fluid.
Compared with the prior art, the invention has the beneficial technical effects that:
the long-chain alkyl acid amide propyl dimethylamine surfactant adopted by the invention is a pH sensitive surfactant, the surface of an anhydride modified nano particle has a carboxyl functional group, a nano fluid formed by the surfactant has certain acidity, the pH value of the solution is adjusted through the concentration of the nano fluid, the long-chain alkyl acid amide propyl dimethylamine surfactant is promoted to be protonated, and the long-chain alkyl acid amide propyl dimethylamine surfactant is wound and crosslinked in the nano fluid to form a long-chain worm-shaped micelle structure and stably exists under a counter ion auxiliary agent. In addition, the anhydride modified nano-particles can also play a role of a reinforcer, the tail ends of micelle molecules can be adsorbed on the surfaces of the nano-particles to form a bridging structure, and the strength of the micelle network structure in the solution can be further enhanced through the double mechanism effects.
Drawings
FIG. 1 is a graph showing the results of steady state shear viscosity testing of a temperature tolerant composite clean fracturing fluid prepared in example 1;
FIG. 2 is a graph showing the results of viscoelasticity tests on the temperature-tolerant composite clean fracturing fluid prepared in example 2;
fig. 3 is a graph showing the results of steady state shear viscosity testing of the temperature resistant composite clean fracturing fluid prepared in example 3.
Detailed Description
The temperature-resistant composite clean fracturing fluid provided by the invention is simple in preparation method, and the colloid-forming structure of the long-chain surfactant is further strengthened by using the anhydride-modified nano silicon dioxide particles, so that the viscoelasticity and the temperature resistance of the clean fracturing fluid are improved, and the application of the clean fracturing fluid in a complex reservoir stratum is widened.
A temperature-resistant composite clean fracturing fluid comprises the following components in percentage by mass:
1-2% of a surfactant; 1-2% of a counter ion auxiliary agent; 1-2% of nano particles; the balance being water.
The preparation method of the temperature-resistant composite clean fracturing fluid comprises the following steps:
(1) dispersing common hydrophilic nano silicon dioxide in an organic solvent by using an ultrasonic cleaner, then adding an anhydride organic substance, and magnetically stirring for 15 hours at room temperature at the rotating speed of 600-.
(2) And (2) putting the anhydride modified nano-particle reaction liquid obtained in the step (1) into a high-speed centrifuge for high-speed centrifugation at 9000 r/min for 30 min, collecting a centrifugation product, washing for 3 times by using ethanol to remove unreacted anhydride organic matters, after the ethanol washing is finished, performing vacuum drying to remove residual organic solvents and ethanol, and grinding the dried solid to obtain the anhydride modified nano-silica particles.
(3) Adding the anhydride modified nano silicon dioxide particles prepared in the step (2) into water, mechanically stirring for 30 minutes under the condition that the rotating speed is 500-600 r/min until the solution is uniform, then placing the solution into an ultrasonic cleaner, and ultrasonically dispersing for 3-4 hours at 50-60 ℃ until the solution is clear and transparent to obtain nano fluid;
(4) and (4) taking the nanofluid prepared in the step (3) as a base fluid, sequentially adding a surfactant and a counter-ion auxiliary agent, uniformly mixing, and then placing into a 50 ℃ water bath kettle to stably stand for 2-3 hours to obtain the temperature-resistant composite clean fracturing fluid.
The present invention will be described in further detail with reference to the accompanying drawings and specific embodiments.
Example 1
A temperature-resistant composite clean fracturing fluid comprises the following components in percentage by mass:
1% of behenamidopropyl dimethylamine; 1% of sodium salicylate; 1% of modified nano particles and the balance of water.
The preparation method of the temperature-resistant composite clean fracturing fluid comprises the following steps:
(1) 2g of a mixture having a particle diameter of 20nm and a specific surface area of 240m2Dispersing the/g common hydrophilic nano silicon dioxide in 200ml of N, N-dimethyl amide by using an ultrasonic cleaner, then adding 2g of maleic anhydride, and magnetically stirring for 15 hours at room temperature at the rotating speed of 600 revolutions per minute to obtain the maleic anhydride modified nano particle reaction liquid.
(2) Putting the maleic anhydride modified nano-particle reaction liquid obtained in the step (1) into a high-speed centrifuge for high-speed centrifugation, wherein the rotating speed is 9000 revolutions per minute, and the centrifugation time is 30 minutes; collecting the centrifugal product, washing with ethanol for 3 times to remove the unreacted maleic anhydride; and after the washing with ethanol is finished, vacuum drying is carried out to remove the residual organic solvent and ethanol, and the dried solid is ground to obtain 2g of maleic anhydride modified nano-silica particles.
(3) Adding 2g of maleic anhydride modified nano silicon dioxide particles into 194g of water, and mechanically stirring for 30 minutes until the solution is uniform, wherein the rotating speed is 500 revolutions per minute; and then placing the solution into an ultrasonic cleaner for ultrasonic dispersion for 3 hours at 50 ℃ until the solution is clear and transparent to obtain the maleic anhydride nanofluid.
(4) And (4) taking the maleic anhydride nanofluid prepared in the step (3) as a base solution, sequentially adding 2g of amidopropyl dimethylamine behenate surfactant and 2g of sodium salicylate, uniformly mixing, and placing into a 50 ℃ water bath kettle to stably stand for 2 hours to obtain the temperature-resistant composite clean fracturing fluid.
The temperature-resistant composite clean fracturing fluid prepared in the embodiment is subjected to a steady-state shear viscosity test: a Haake Mars 60 rheometer is adopted to test the steady-state shear viscosity of the temperature-resistant composite clean fracturing fluid at 75 ℃, and the test result is shown in figure 1.
As can be seen from fig. 1, the shear viscosity of the temperature-resistant composite clean fracturing fluid prepared in example 1 can maintain a high viscosity at a low shear rate, which is above 2000mPa · s, and a viscosity plateau occurs, since the network structure of the wormlike micelles in the fracturing fluid can be relatively stable at the low shear viscosity. As the shear rate increases, the fracturing fluid viscosity begins to decrease, indicating a shear thinning phenomenon. This is because the high shear causes the micelle network to break down.
Example 2
A temperature-resistant composite clean fracturing fluid comprises the following components in percentage by mass:
2% of stearic acid amide propyl dimethylamine; sodium p-toluenesulfonate 1.5%; 2% of modified nano particles and the balance of water.
The preparation method of the temperature-resistant composite clean fracturing fluid comprises the following steps:
(1) 4g of a polymer having a particle diameter of 25nm and a specific surface area of 300m2Dispersing/g common hydrophilic nano silicon dioxide in 200ml toluene by using an ultrasonic cleaner, then adding 4.5g trimellitic anhydride, magnetically stirring for 15 hours at room temperature at the rotating speed of 650 revolutions per minute to obtain trimellitic anhydride modified nano particles, and reactingAnd (4) liquid.
(2) Putting the trimellitic anhydride modified nanoparticle reaction solution obtained in the step (1) into a high-speed centrifuge for high-speed centrifugation at 9000 revolutions per minute for 30 minutes; collecting the centrifugal product, washing with ethanol for 3 times to remove the incompletely reacted trimellitic anhydride; and after the ethanol washing is finished, carrying out vacuum drying to remove the residual organic solvent and ethanol, and grinding the dried solid to obtain 4g of trimellitic anhydride modified nano-silica particles.
(3) Adding 4g of trimellitic anhydride modified nano silica particles into 189g of water, and mechanically stirring for 30 minutes until the solution is uniform, wherein the rotating speed is 550 revolutions per minute; then the solution is placed into an ultrasonic cleaner for ultrasonic dispersion for 3 hours at 50 ℃ until the solution is clear and transparent, and the nano-fluid of the trimellitic anhydride is obtained.
(4) And (3) taking the trimellitic anhydride nanofluid prepared in the step (3) as a base solution, sequentially adding 4g of stearic acid amide propyl dimethylamine surfactant and 3g of sodium p-toluenesulfonate, uniformly mixing, and placing into a 50 ℃ water bath kettle to stably stand for 2.5 hours to obtain the temperature-resistant composite clean fracturing fluid.
The temperature-resistant composite clean fracturing fluid prepared in the embodiment is subjected to a steady-state shear viscosity test: a Haake Mars 60 rheometer is adopted to test the steady-state shear viscosity of the temperature-resistant composite clean fracturing fluid at 80 ℃, and the test result is shown in figure 2. As can be seen from fig. 2, the temperature-resistant composite clean fracturing fluid prepared in example 2 shows good viscoelastic properties.
Example 3
A temperature-resistant composite clean fracturing fluid comprises the following components in percentage by mass:
erucamidopropyl dimethylamine 1.5%; 2 percent of sodium dodecyl sulfate; 1.5% of modified nano particles and the balance of water.
The preparation method of the temperature-resistant composite clean fracturing fluid comprises the following steps:
(1) 3g of a material having a particle diameter of 15nm and a specific surface area of 380m2The/g ordinary hydrophilic nano-silica was dispersed in 200ml of cyclohexane by an ultrasonic cleaner, and thenAdding 4g succinic anhydride, and magnetically stirring at room temperature for 15 hours at the rotating speed of 700 r/min to obtain succinic anhydride modified nano-particle reaction liquid.
(2) Putting the succinic anhydride modified nano-particle reaction liquid obtained in the step (1) into a high-speed centrifuge for high-speed centrifugation at 9000 revolutions per minute for 30 minutes; collecting the centrifugal product, washing with ethanol for 3 times to remove unreacted succinic anhydride; and after washing with ethanol, performing vacuum drying to remove the residual organic solvent and ethanol, and grinding the dried solid to obtain 3g of succinic anhydride modified nano-silica particles.
(3) Adding 3g of succinic anhydride modified nano silicon dioxide particles into 190g of water, and mechanically stirring for 30 minutes until the solution is uniform, wherein the rotating speed is 600 revolutions per minute; and then placing the solution into an ultrasonic cleaner for ultrasonic dispersion for 3 hours at 50 ℃ until the solution is clear and transparent to obtain the succinic anhydride nanofluid.
(4) And (3) sequentially adding 3g of erucamidopropyldimethylamine surfactant and 4g of sodium dodecyl sulfate into the succinic anhydride nano fluid prepared in the step (3) serving as a base fluid, uniformly mixing, and placing the mixture into a 50 ℃ water bath kettle to stably stand for 2.5 hours to obtain the temperature-resistant composite clean fracturing fluid.
The temperature-resistant composite clean fracturing fluid prepared in the embodiment is subjected to a steady-state shear viscosity test: the temperature-resistant composite clean fracturing fluid is tested by adopting a Haake Mars 60 rheometer at 85 ℃ for 170s-1The shear viscosity at shear rate is shown in FIG. 3 as a function of time. As can be seen from fig. 3, the temperature-resistant composite clean fracturing fluid prepared in example 3 still has a viscosity of 80mPa · s or more after shearing for 2 hours.
Although the invention has been described in detail above with reference to a general description and specific examples, it will be apparent to one skilled in the art that modifications or improvements may be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.
Claims (5)
1. The temperature-resistant composite clean fracturing fluid is characterized by comprising the following components in percentage by mass:
1-2% of a surfactant; 1-2% of a counter ion auxiliary agent; 1-2% of nano particles; the balance of water;
the surfactant is one of behenamidopropyl dimethylamine, stearic acid amidopropyl dimethylamine, palmitic acid amidopropyl dimethylamine or erucic acid amidopropyl dimethylamine;
the nanoparticles are modified nanoparticles; the modified nano-particles are hydrophilic nano-silica particles which are subjected to surface modification by using anhydride organic matters; the preparation method comprises the following steps:
A. dispersing common hydrophilic nano silicon dioxide in an organic solvent by using an ultrasonic cleaner, then adding an anhydride organic substance, and magnetically stirring for 15 hours at room temperature at the rotating speed of 600-700rpm to obtain an anhydride modified nano particle reaction solution;
B. b, placing the anhydride modified nano-particle reaction solution obtained in the step A into a high-speed centrifuge for high-speed centrifugation at 9000 rpm for 30 minutes, collecting a centrifugal product, washing the centrifugal product with ethanol for 3 times to remove unreacted anhydride organic matters, after the ethanol washing is finished, performing vacuum drying to remove residual organic solvents and ethanol, and grinding the dried solid to obtain anhydride modified nano-silica particles;
the counter ion auxiliary agent is one of sodium salicylate, sodium nitrate, sodium maleate, sodium dodecyl sulfate, sodium dodecyl benzene sulfonate or sodium p-toluenesulfonate.
2. The temperature-resistant composite clean fracturing fluid of claim 1, wherein: the acid anhydride organic matter is one of succinic anhydride, glutaric anhydride, maleic anhydride, trimellitic anhydride or phthalic anhydride.
3. The temperature-resistant composite clean fracturing fluid of claim 1, wherein: in the step A, the organic solvent is any one of toluene, cyclohexane or N, N-dimethyl amide.
4. The temperature-resistant composite clean fracturing fluid of claim 1, wherein: in the step A, the mass ratio of the anhydride organic matter to the common hydrophilic nano silicon dioxide particles is 3-4: 3.
5. The method for preparing the temperature-resistant composite clean fracturing fluid of any one of claims 1 to 4, which is characterized by comprising the following steps:
(1) adding the nano particles into water, mechanically stirring for 30 minutes under the condition of the rotation speed of 500 plus 600 revolutions per minute until the solution is uniform, then placing the solution into an ultrasonic cleaner, and ultrasonically dispersing for 3 hours at 50 ℃ until the solution is clear and transparent to obtain a nano fluid;
(2) and (2) taking the nanofluid prepared in the step (1) as a base fluid, sequentially adding a surfactant and a counter-ion auxiliary agent, uniformly mixing, and then placing into a 50 ℃ water bath kettle to stably stand for 2-2.5 hours to obtain the temperature-resistant composite clean fracturing fluid.
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| CN109337663A (en) * | 2018-11-19 | 2019-02-15 | 中国石油集团川庆钻探工程有限公司工程技术研究院 | Low permeability reservoir continuous mixed displacement of reservoir oil type fracturing fluid and its preparation method and application |
| CN110257042B (en) * | 2019-07-06 | 2021-06-04 | 西南石油大学 | Clean fracturing fluid for automatic reservoir gel breaking and preparation method thereof |
| CN110257043B (en) * | 2019-07-06 | 2021-06-04 | 西南石油大学 | Stimulus-response type clean fracturing fluid and preparation method thereof |
| CN110373173A (en) * | 2019-07-23 | 2019-10-25 | 孙国平 | A kind of repeatable crosslinking clean fracturing fluid thickener of high temperature resistant |
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| CN116042206B (en) * | 2021-10-28 | 2024-04-16 | 中国石油天然气集团有限公司 | Viscoelastic micro-nano thickener for oil-gas well fracturing, fracturing fluid and preparation method |
| CN114106810B (en) * | 2021-11-05 | 2023-01-03 | 中国地质大学（北京） | Nano silicon dioxide, nano composite slickwater fracturing fluid, preparation method and application |
| CN114956495B (en) * | 2022-06-23 | 2023-04-25 | 山东大学 | PH response type compound surfactant cleaning solution and treatment method of oily sludge |
| CN115287052B (en) * | 2022-08-19 | 2024-03-08 | 中国石油大学(华东) | Carbon point compound oil displacement system based on interface regulation and control and preparation method and application thereof |
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| CN108285783A (en) | 2018-07-17 |
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