Preparation method of thickening agent for oil extraction fracturing

By preparing a mixed reaction of water phase and oil phase, the problem of thickener failure under high temperature and high salt conditions is solved, and a thickener with excellent shear resistance, temperature resistance and salt resistance is provided, which improves oil and gas extraction efficiency and reduces environmental risks.

CN120737274APending Publication Date: 2025-10-03DAQING HUAYING CHEM IND CO LTD
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Patent Information

Application Number
CN202511087157.7
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-08-05
Publication Date
2025-10-03

AI Technical Summary

Technical Problem

Existing thickeners are prone to failure under high temperature, high salinity or oil-water phase distribution conditions, contain toxic ingredients, are harmful to the environment, and have complex synthesis processes and high costs.

Method used

Acrylamide, acrylic acid, Tween-80, isopropylamine dodecylbenzenesulfonate, azobisisobutylimidazoline hydrochloride and other substances are used to prepare the water phase, and 0# diesel, methyl methacrylate, butadiene and other substances are used to prepare the oil phase. The thickener is prepared through mixing, stirring and heating reaction.

Benefits of technology

The prepared thickener has significantly better shear resistance, temperature resistance, salt resistance and suspended sand properties than existing thickeners, with improved viscosity and suspended sand rate, and is environmentally friendly and cost-effective.

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Abstract

The invention belongs to the field of oilfield chemical treatment agents, and particularly relates to a preparation method of a thickening agent for oil extraction fracturing, which comprises the following steps: 1, uniformly mixing 25 parts of acrylamide, 15 parts of acrylic acid, 4 parts of Tween-80, 1.5 parts of dodecyl benzene sulfonic acid isopropylamine salt, 90 parts of deionized water and 2.5 parts of azodiisobutylimidazoline hydrochloride to obtain a water phase; 2, uniformly mixing 45 parts of 0 # diesel oil, 14 parts of methyl methacrylate, 7 parts of butadiene, 7 parts of diacetone acrylamide and 6 parts of butanol polyoxypropylene ether to obtain an oil phase; and 3, putting the oil phase into a reaction kettle, adding the water phase into the oil phase, uniformly stirring at the rotating speed of a motor of 9000rpm for 30 minutes, adjusting the rotating speed to 700rpm, introducing nitrogen for 30 minutes, heating to 535 DEG C, stirring for reacting for 10 hours, and cooling to obtain the fracturing fluid thickening agent for oil extraction. The shearing resistance, the temperature resistance, the salt resistance and the sand suspending property of the thickening agent are superior to those of the existing thickening agent.
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Description

Technical Field

[0001] The invention belongs to the field of oilfield chemical treatment agents, and in particular relates to a method for preparing a thickener for oil production and fracturing. Background Art

[0002] Oilfield fracturing cleaning thickeners are polymer additives used to increase the viscosity and improve the rheological properties of aqueous systems. They are a key component of fracturing fluids. As oil and natural gas extraction increasingly relies on hydraulic fracturing technology, the performance of cleaning and thickening agents directly impacts the rheological properties and stability of fracturing fluids, as well as their ability to suspend solid particles in oil and gas wells, thereby improving oil and gas extraction efficiency. Traditional oilfield fracturing thickeners are typically composed of natural or synthetic polymers and surfactants. Synthetic polymers offer excellent thickening properties in water, with superior temperature and shear resistance, strong thickening capacity, excellent sand suspension and gel breaking properties, and bacterial resistance, outperforming natural polymers in all respects.

[0003] Existing thickeners have defects. Under high temperature, high salinity or oil-water phase distribution conditions, thickeners are easily ineffective, resulting in reduced application effectiveness in oil fields. Many traditional thickeners contain toxic and harmful ingredients, posing potential hazards to the environment and ecosystems. The raw materials of some high-efficiency thickeners are expensive and the synthesis process is complex. In order to overcome these shortcomings, the development of more efficient, stable, environmentally friendly and cost-effective thickeners has become a technical problem that needs to be solved urgently. Summary of the Invention

[0004] In order to solve the above problems, the present invention provides a method for preparing a thickener for oil fracturing. The thickener prepared by the method has significantly better shear resistance, temperature resistance, salt resistance and sand suspension than existing thickeners.

[0005] The technical solution adopted by the present invention is: a method for preparing a thickener for oil fracturing, the preparation method comprising the following steps: Step 1: put 20-30 parts of acrylamide, 10-20 parts of acrylic acid, 3-5 parts of Tween-80, 1-2 parts of dodecylbenzenesulfonic acid isopropylamine salt, 80-100 parts of deionized water, and 2-3 parts of azobisisobutylimidazoline hydrochloride into a preparation tank and mix them evenly to obtain an aqueous phase.

[0006] Step 2: Combine 40-50 portions of # Diesel oil, 10-18 parts of methyl methacrylate, 6-8 parts of butadiene, 5-9 parts of diacetone acrylamide and 4-8 parts of butanol polyoxypropylene ether are put into a preparation tank and mixed evenly to obtain an oil phase.

[0007] Step 3: Place the oil phase obtained in step 2 in a reactor, then add the water phase obtained in step 1 to the oil phase and stir evenly. The motor speed is 8000-10000 rpm. After stirring for 30 minutes, the speed is adjusted to 600-800 rpm, and nitrogen is introduced for 30 minutes. Heat to 50°C-55°C, stir for 8-12 hours, and then cool to obtain a fracturing fluid thickener for oil production.

[0008] Furthermore, the preparation method of the thickener for oil fracturing is as follows: Step 1: 25 parts of acrylamide, 15 parts of acrylic acid, 4 parts of Tween-80, 1.5 parts of dodecylbenzenesulfonic acid isopropylamine salt, 90 parts of deionized water, and 2.5 parts of azobisisobutylimidazoline hydrochloride are put into a preparation tank and mixed evenly to obtain an aqueous phase.

[0009] Step 2: 45 portions of 0 # Diesel oil, 14 parts of methyl methacrylate, 7 parts of butadiene, 7 parts of diacetone acrylamide and 6 parts of butanol polyoxypropylene ether were put into a preparation tank and mixed evenly to obtain an oil phase.

[0010] Step 3: Place the oil phase obtained in step 2 in a reactor, then add the water phase obtained in step 1 to the oil phase and stir evenly. The motor speed is 9000 rpm. After stirring for 30 minutes, the speed is adjusted to 700 rpm, and nitrogen is introduced for 30 minutes. Heat to 53°C, stir and react for 10 hours, and then cool to obtain a fracturing fluid thickener for oil production.

[0011] Furthermore, the preparation method of the thickener for oil fracturing is as follows: Step 1: put 20 parts of acrylamide, 10 parts of acrylic acid, 3 parts of Tween-80, 1 part of dodecylbenzenesulfonic acid isopropylamine salt, 80 parts of deionized water, and 2 parts of azobisisobutylimidazoline hydrochloride into a preparation tank and mix well to obtain an aqueous phase.

[0012] Step 2: 40 portions of 0 # Diesel oil, 10 parts of methyl methacrylate, 6 parts of butadiene, 5 parts of diacetone acrylamide and 4 parts of butanol polyoxypropylene ether were put into a preparation tank and mixed evenly to obtain an oil phase.

[0013] Step 3: Place the oil phase obtained in step 2 in a reactor, then add the water phase obtained in step 1 to the oil phase and stir evenly. The motor speed is 8000 rpm. After stirring for 30 minutes, the speed is adjusted to 600 rpm, and nitrogen is introduced for 30 minutes. Heat to 50°C, stir and react for 8 hours, and then cool to obtain a fracturing fluid thickener for oil production.

[0014] Furthermore, the preparation method of the thickener for oil fracturing is as follows: Step 1: 30 parts of acrylamide, 20 parts of acrylic acid, 5 parts of Tween-80, 2 parts of dodecylbenzenesulfonic acid isopropylamine salt, 100 parts of deionized water, and 3 parts of azobisisobutylimidazoline hydrochloride are put into a preparation tank and mixed evenly to obtain an aqueous phase.

[0015] Step 2: 50 portions of 0 # Diesel oil, 18 parts of methyl methacrylate, 8 parts of butadiene, 9 parts of diacetone acrylamide and 8 parts of butanol polyoxypropylene ether were put into a preparation tank and mixed evenly to obtain an oil phase.

[0016] Step 3: Place the oil phase obtained in step 2 in a reactor, then add the water phase obtained in step 1 to the oil phase and stir evenly. The motor speed is 10,000 rpm. After stirring for 30 minutes, the speed is adjusted to 800 rpm, and nitrogen is introduced for 30 minutes. Heat to 55°C, stir and react for 12 hours, and then cool to obtain a fracturing fluid thickener for oil production.

[0017] The present invention provides a method for preparing a thickener for oil fracturing. The resulting thickener exhibits significantly superior shear resistance, temperature resistance, salt tolerance, and sand suspension properties compared to existing thickeners. The shear resistance viscosity is above 85 mPa·s, the temperature resistance viscosity is above 63 mPa·s, the salt resistance viscosity is above 91 mPa·s, the sand suspension capacity is above 383 mL, and the sand suspension rate is above 95.75%. DETAILED DESCRIPTION Example 1

[0018] The preparation method of a thickener for oil fracturing comprises the following steps: Step 1: 25 parts of acrylamide, 15 parts of acrylic acid, 4 parts of Tween-80, 1.5 parts of dodecylbenzenesulfonic acid isopropylamine salt, 90 parts of deionized water, and 2.5 parts of azobisisobutylimidazoline hydrochloride are put into a preparation tank and mixed evenly to obtain an aqueous phase.

[0019] Step 2: 45 portions of 0 # Diesel oil, 14 parts of methyl methacrylate, 7 parts of butadiene, 7 parts of diacetone acrylamide and 6 parts of butanol polyoxypropylene ether were put into a preparation tank and mixed evenly to obtain an oil phase.

[0020] Step 3: Place the oil phase obtained in step 2 in a reactor, then add the water phase obtained in step 1 to the oil phase and stir evenly. The motor speed is 8000-10000 rpm. After stirring for 30 minutes, the speed is adjusted to 600-800 rpm, and nitrogen is introduced for 30 minutes. Heat to 50°C-55°C, stir for 10 hours, and then cool to obtain a fracturing fluid thickener for oil production. Example 2

[0021] The preparation method of a thickener for oil fracturing comprises the following steps: Step 1: put 20 parts of acrylamide, 10 parts of acrylic acid, 3 parts of Tween-80, 1 part of dodecylbenzenesulfonic acid isopropylamine salt, 80 parts of deionized water, and 2 parts of azobisisobutylimidazoline hydrochloride into a preparation tank and mix well to obtain an aqueous phase.

[0022] Step 2: 40 portions of 0 # Diesel oil, 10 parts of methyl methacrylate, 6 parts of butadiene, 5 parts of diacetone acrylamide and 4 parts of butanol polyoxypropylene ether were put into a preparation tank and mixed evenly to obtain an oil phase.

[0023] Step 3: Place the oil phase obtained in step 2 in a reactor, then add the water phase obtained in step 1 to the oil phase and stir evenly. The motor speed is 8000-10000 rpm. After stirring for 30 minutes, the speed is adjusted to 600-800 rpm, and nitrogen is introduced for 30 minutes. Heat to 50°C-55°C, stir for 8 hours, and then cool to obtain a fracturing fluid thickener for oil production. Example 3

[0024] The preparation method of a thickener for oil fracturing comprises the following steps: Step 1: 30 parts of acrylamide, 20 parts of acrylic acid, 5 parts of Tween-80, 2 parts of dodecylbenzenesulfonic acid isopropylamine salt, 100 parts of deionized water, and 3 parts of azobisisobutylimidazoline hydrochloride are put into a preparation tank and mixed evenly to obtain an aqueous phase.

[0025] Step 2: 50 portions of 0 # Diesel oil, 18 parts of methyl methacrylate, 8 parts of butadiene, 9 parts of diacetone acrylamide and 8 parts of butanol polyoxypropylene ether were put into a preparation tank and mixed evenly to obtain an oil phase.

[0026] Step 3: Place the oil phase obtained in step 2 in a reactor, then add the water phase obtained in step 1 to the oil phase and stir evenly. The motor speed is 8000-10000 rpm. After stirring for 30 minutes, the speed is adjusted to 600-800 rpm, and nitrogen is introduced for 30 minutes. Heat to 50°C-55°C, stir and react for 12 hours, and then cool to obtain a fracturing fluid thickener for oil production. Example 4

[0027] Performance testing of thickeners 1. Prepare the thickener of each embodiment (Example 1-3) into a thickener solution with a mass fraction of 0.3%, and heat it for 5-10 seconds at room temperature. -1 The shear rate was 600s, and the viscosity of the fracturing fluid was tested to evaluate the shear resistance.

[0028] 2. Prepare the thickener of each embodiment into a thickener solution with a mass fraction of 0.3%, and -1Shear rate and viscosity of fracturing fluid were measured at 140℃ to evaluate temperature resistance.

[0029] 3. The thickeners of each embodiment were prepared into a thickener solution with a mass fraction of 0.4%. The viscosity of the fracturing fluid jelly after salt treatment with sodium chloride with a mass fraction of 10 g / L was tested to evaluate the salt resistance.

[0030] 4. Prepare the thickener of each example into a 0.3% thickener solution by mass, add 400 mL into a 500 mL graduated cylinder, add 20% 60 mesh quartz sand, stir evenly for 20 minutes, and then measure the volume of the suspended sand.

[0031] The results are shown in Table 1: Table 1

[0032] The above results show that the shear resistance, temperature resistance, salt resistance, and sand suspension of each embodiment are superior to those of the existing thickener. The shear resistance viscosity is above 85 MPa·s, the temperature resistance viscosity is higher than 63 MPa·s, the salt resistance viscosity is higher than 91 MPa·s, the sand suspension is higher than 383 mL, and the suspended sand rate is higher than 95.75%.

[0033] The above embodiments are only some exemplary embodiments of the present invention, not all embodiments, and are not intended to limit the present invention. The scope of protection of the present invention is defined by the claims. Those skilled in the art may make various modifications or equivalent substitutions to the present invention within the spirit and scope of protection of the present invention, and such modifications or equivalent substitutions shall also be deemed to fall within the scope of protection of the present invention.

Claims

1. A method for preparing a thickener for oil fracturing, characterized in that: The preparation method comprises the following steps: Step 1: put 20-30 parts of acrylamide, 10-20 parts of acrylic acid, 3-5 parts of Tween-80, 1-2 parts of dodecylbenzenesulfonic acid isopropylamine salt, 80-100 parts of deionized water, and 2-3 parts of azobisisobutylimidazoline hydrochloride into a preparation tank and mix well to obtain an aqueous phase; Step 2: Combine 40-50 portions of # Diesel oil, 10-18 parts of methyl methacrylate, 6-8 parts of butadiene, 5-9 parts of diacetone acrylamide, and 4-8 parts of polyoxypropylene butanol ether are put into a preparation tank and mixed evenly to obtain an oil phase; Step 3: Place the oil phase obtained in step 2 in a reactor, then add the water phase obtained in step 1 to the oil phase and stir evenly. The motor speed is 8000-10000 rpm. After stirring for 30 minutes, the speed is adjusted to 600-800 rpm, and nitrogen is introduced for 30 minutes. Heat to 50°C-55°C, stir for 8-12 hours, and then cool to obtain a fracturing fluid thickener for oil production.

2. The method for preparing a thickener for oil fracturing according to claim 1, wherein: The preparation method comprises the following steps: Step 1: put 25 parts of acrylamide, 15 parts of acrylic acid, 4 parts of Tween-80, 1.5 parts of dodecylbenzenesulfonic acid isopropylamine salt, 90 parts of deionized water, and 2.5 parts of azobisisobutylimidazoline hydrochloride into a mixing tank and mix well to obtain an aqueous phase; Step 2: 45 portions of 0 # Diesel oil, 14 parts of methyl methacrylate, 7 parts of butadiene, 7 parts of diacetone acrylamide, and 6 parts of polyoxypropylene butanol ether are put into a preparation tank and mixed evenly to obtain an oil phase; Step 3: Place the oil phase obtained in step 2 in a reactor, then add the water phase obtained in step 1 to the oil phase and stir evenly. The motor speed is 8000-10000 rpm. After stirring for 30 minutes, the speed is adjusted to 600-800 rpm, and nitrogen is introduced for 30 minutes. Heat to 50°C-55°C, stir for 10 hours, and then cool to obtain a fracturing fluid thickener for oil production.

3. The method for preparing a thickener for oil fracturing according to claim 1, wherein: The preparation method comprises the following steps: Step 1: put 20 parts of acrylamide, 10 parts of acrylic acid, 3 parts of Tween-80, 1 part of dodecylbenzenesulfonic acid isopropylamine salt, 80 parts of deionized water, and 2 parts of azobisisobutylimidazoline hydrochloride into a preparation tank and mix well to obtain an aqueous phase; Step 2: 40 portions of 0 # Diesel oil, 10 parts of methyl methacrylate, 6 parts of butadiene, 5 parts of diacetone acrylamide, and 4 parts of polyoxypropylene butanol ether were put into a preparation tank and mixed evenly to obtain an oil phase; Step 3: Place the oil phase obtained in step 2 in a reactor, then add the water phase obtained in step 1 to the oil phase and stir evenly. The motor speed is 8000-10000 rpm. After stirring for 30 minutes, the speed is adjusted to 600-800 rpm, and nitrogen is introduced for 30 minutes. Heat to 50°C-55°C, stir for 8 hours, and then cool to obtain a fracturing fluid thickener for oil production.

4. The method for preparing a thickener for oil fracturing according to claim 1, wherein: The preparation method comprises the following steps: Step 1: 30 parts of acrylamide, 20 parts of acrylic acid, 5 parts of Tween-80, 2 parts of isopropylamine dodecylbenzenesulfonate, 100 parts of deionized water, and 3 parts of azobisisobutylimidazoline hydrochloride are put into a preparation tank and mixed uniformly to obtain an aqueous phase; Step 2: 50 portions of 0 # Diesel oil, 18 parts of methyl methacrylate, 8 parts of butadiene, 9 parts of diacetone acrylamide, and 8 parts of polyoxypropylene butanol ether were put into a preparation tank and mixed evenly to obtain an oil phase; Step 3: Place the oil phase obtained in step 2 in a reactor, then add the water phase obtained in step 1 to the oil phase and stir evenly. The motor speed is 8000-10000 rpm. After stirring for 30 minutes, the speed is adjusted to 600-800 rpm, and nitrogen is introduced for 30 minutes. Heat to 50°C-55°C, stir and react for 12 hours, and then cool to obtain a fracturing fluid thickener for oil production.

5. The method for preparing a thickener for oil fracturing according to claim 2, wherein: The preparation method comprises the following steps: In step 3, the motor speed is 9000 rpm. After stirring for 30 minutes, the speed is adjusted to 700 rpm, and nitrogen is introduced for 30 minutes, and then the temperature is heated to 53°C.

6. The method for preparing a thickener for oil fracturing according to claim 3, wherein: The preparation method comprises the following steps: In step 3, the motor speed is 8000 rpm. After stirring for 30 minutes, the speed is adjusted to 600 rpm, and nitrogen is introduced for 30 minutes, and then the temperature is heated to 50°C.

7. The method for preparing a thickener for oil fracturing according to claim 4, wherein: In step 3, the motor speed is 10000 rpm. After stirring for 30 minutes, the speed is adjusted to 800 rpm, and nitrogen is introduced for 30 minutes, and then the temperature is heated to 55°C.