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CN104152134A - Medium and high temperature fracturing fluid and preparation method thereof - Google Patents

Medium and high temperature fracturing fluid and preparation method thereof Download PDF

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CN104152134A
CN104152134A CN201410328621.2A CN201410328621A CN104152134A CN 104152134 A CN104152134 A CN 104152134A CN 201410328621 A CN201410328621 A CN 201410328621A CN 104152134 A CN104152134 A CN 104152134A
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mass fraction
aqueous solution
sodium
fracturing fluid
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孟江燕
王云英
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Nanchang Hangkong University
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    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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    • C09K8/00Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
    • C09K8/60Compositions for stimulating production by acting on the underground formation
    • C09K8/602Compositions for stimulating production by acting on the underground formation containing surfactants
    • C09K8/604Polymeric surfactants
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    • C09K8/00Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
    • C09K8/60Compositions for stimulating production by acting on the underground formation
    • C09K8/62Compositions for forming crevices or fractures
    • C09K8/66Compositions based on water or polar solvents
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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    • C09K8/00Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
    • C09K8/60Compositions for stimulating production by acting on the underground formation
    • C09K8/84Compositions based on water or polar solvents
    • C09K8/86Compositions based on water or polar solvents containing organic compounds
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Abstract

本发明公开了一种中高温压裂液及其制备方法,压裂液主要包括:聚丙烯酸钠、聚丙烯酰胺、十六烷基二羟乙基甜菜碱、羟基苯甲酸钠、乙二醇、氯化钠,其制备方法包括聚合物阳离子表面活性剂的合成,并与两性表面活性剂、电介质、助溶剂和水复配为压裂液。本发明的优点是:该压裂液可在90℃到110℃温度范围保持良好的悬砂性能。The invention discloses a medium-high temperature fracturing fluid and a preparation method thereof. The fracturing fluid mainly includes: sodium polyacrylate, polyacrylamide, cetyl dihydroxyethyl betaine, sodium hydroxybenzoate, ethylene glycol, chlorine Sodium chloride, the preparation method of which includes the synthesis of polymer cationic surfactants, and compounding with amphoteric surfactants, dielectrics, co-solvents and water to form fracturing fluids. The invention has the advantages that: the fracturing fluid can maintain good sand suspension performance in the temperature range of 90°C to 110°C.

Description

一种中高温压裂液及其制备方法A medium-high temperature fracturing fluid and its preparation method

技术领域 technical field

本发明涉及一种油气田开发过程中压裂措施的一种压裂液,具体涉及一种可在90~110 ℃温度条件下使用的中高温压裂液及其制备方法。 The invention relates to a fracturing fluid for fracturing measures in the process of oil and gas field development, in particular to a medium-high temperature fracturing fluid that can be used at a temperature of 90-110 °C and a preparation method thereof.

背景技术 Background technique

压裂作为油气田开发增产的措施已经得到迅速发展和广泛应用,压裂液是压裂技术的主要组成部分。 Fracturing has been rapidly developed and widely used as a measure to increase production in oil and gas field development, and fracturing fluid is the main component of fracturing technology.

本发明制备的低分子量聚丙烯酸钠为聚合物类表面活性剂,再与两性表面活性剂十六烷基二羟乙基甜菜碱复配,可以在碱性环境下吸附在气/液表面而降低水溶液的表面张力、聚集形成胶团以及良好的增溶能力。 The low-molecular-weight sodium polyacrylate prepared by the present invention is a polymer surfactant, and then compounded with the amphoteric surfactant cetyl dihydroxyethyl betaine, which can be adsorbed on the gas/liquid surface in an alkaline environment to reduce the Surface tension of aqueous solution, aggregation to form micelles and good solubilization ability.

发明内容 Contents of the invention

本发明的目的在于提供一种中高温压裂液及其制备方法,按本发明的制备方法得到的中高温压裂液是一种在中高温下保持优异的粘度特性和表面活性的压裂液,可用于油气田压裂增产。 The purpose of the present invention is to provide a medium-high temperature fracturing fluid and its preparation method. The medium-high temperature fracturing fluid obtained according to the preparation method of the present invention is a fracturing fluid that maintains excellent viscosity characteristics and surface activity at medium and high temperatures , can be used for oil and gas field fracturing stimulation.

本发明是这样来实现的,一种中高温压裂液,其特征在于:分子量1000~2000的聚丙烯酸钠的质量分数5%,分子量大于1×107的聚丙烯酰胺的质量分数5%,十六烷基二羟乙基甜菜碱的质量分数3%,氯化钠的质量分数2%,乙二醇的质量分数1%,羟基苯甲酸钠的质量分数0.1%,余量为水。 The present invention is achieved in this way, a medium-high temperature fracturing fluid, characterized in that: the mass fraction of sodium polyacrylate with a molecular weight of 1000-2000 is 5%, the mass fraction of polyacrylamide with a molecular weight greater than 1× 107 is 5%, The mass fraction of cetyl dihydroxyethyl betaine is 3%, the mass fraction of sodium chloride is 2%, the mass fraction of ethylene glycol is 1%, the mass fraction of sodium hydroxybenzoate is 0.1%, and the balance is water.

本发明所述中高温压裂液的制备方法,其特征在于方法步骤为: The preparation method of the medium-high temperature fracturing fluid of the present invention is characterized in that the method steps are:

1、聚丙烯酸钠的制备; 1. Preparation of sodium polyacrylate;

(1)把质量分数为30%的丙烯酸钠溶于质量分数为60%的水中,配制成水溶液; (1) Dissolve sodium acrylate with a mass fraction of 30% in water with a mass fraction of 60% to prepare an aqueous solution;

(2)把质量分数为4%的碳酸钠,加入步骤(1)配制的水溶液中; (2) adding mass fraction of 4% sodium carbonate to the aqueous solution prepared in step (1);

(3)把质量分数为1.5%的十二硫醇和1.5%的过硫酸钾,加入步骤(1)配制的水溶液中; (3) adding 1.5% dodecanethiol and 1.5% potassium persulfate to the aqueous solution prepared in step (1) with a mass fraction;

(4)把步骤(1)、(2)和(3)所配制的水溶液注入容器中,通入氮气3~5分钟后,密闭容器; (4) Pour the aqueous solution prepared in steps (1), (2) and (3) into the container, and after 3 to 5 minutes of nitrogen gas, airtight the container;

(5)置于58±2 ℃的水浴中5 小时以上; (5) Place in a water bath at 58±2°C for more than 5 hours;

(6)将淡黄色粘稠状产物洗涤后,置于真空干燥箱干燥,得到分子量为1000~2000的聚丙烯酸钠。 (6) Wash the pale yellow viscous product and dry it in a vacuum oven to obtain sodium polyacrylate with a molecular weight of 1000-2000.

2、聚丙烯酰胺的制备; 2. Preparation of polyacrylamide;

(1)把质量分数为24%的丙烯酰胺溶于质量分数为73%的水中,配制成水溶液; (1) Dissolve acrylamide with a mass fraction of 24% in water with a mass fraction of 73% to prepare an aqueous solution;

(2)把质量分数为2.5%的碳酸钠,加入步骤(1)配制的水溶液中; (2) adding mass fraction of 2.5% sodium carbonate to the aqueous solution prepared in step (1);

(3)把质量分数为0.25%的碳酰二胺脲和0.25%的过硫酸铵,加入步骤(1)配制的水溶液中; (3) Add carbodiamide urea and 0.25% ammonium persulfate with a mass fraction of 0.25% to the aqueous solution prepared in step (1);

(4)把步骤(1)、(2)和(3)所配制的水溶液注入容器中,通入氮气5分钟后,密闭容器; (4) Pour the aqueous solution prepared in steps (1), (2) and (3) into the container, and after passing nitrogen gas for 5 minutes, seal the container;

(5)置于20±2 ℃的水浴中8 小时以上; (5) Place in a water bath at 20±2°C for more than 8 hours;

(6)将透明粘稠状产物洗涤后,置于真空干燥箱干燥,得到分子量为大于1×107的聚丙烯酰胺。  (6) Wash the transparent viscous product and dry it in a vacuum oven to obtain polyacrylamide with a molecular weight greater than 1×10 7 .

3、压裂液的配制; 3. Preparation of fracturing fluid;

(1)把质量分数1%乙二醇加入水中; (1) Add 1% ethylene glycol by mass fraction to water;

(2)加入质量分数5%聚丙烯酸钠、质量分数5%聚丙烯酰胺和质量分数3%十六烷基二羟乙基甜菜碱,搅拌直至形成均匀透明的溶液; (2) Add 5% sodium polyacrylate, 5% polyacrylamide and 3% hexadecyl dihydroxyethyl betaine, and stir until a uniform and transparent solution is formed;

(3)加入质量分数2%氯化钠和质量分数0.1%羟基苯甲酸钠,搅拌均匀,得到压裂液。 (3) Add 2% sodium chloride by mass fraction and 0.1% sodium hydroxybenzoate by mass fraction, and stir evenly to obtain fracturing fluid.

具体实施方式 Detailed ways

实施例一Embodiment one

1、聚丙烯酸钠的制备 1. Preparation of sodium polyacrylate

(1)把300 g的丙烯酸钠溶于质量分数为600 g的水中,配制成水溶液; (1) Dissolve 300 g of sodium acrylate in water with a mass fraction of 600 g to prepare an aqueous solution;

(2)把4 g的碳酸钠,加入步骤(1)配制的水溶液中; (2) Add 4 g of sodium carbonate to the aqueous solution prepared in step (1);

(3)把质量分数为1.5 g的十二硫醇和1.5 g 的过硫酸钾,加入步骤(1)配制的水溶液中; (3) Add 1.5 g of dodecanethiol and 1.5 g of potassium persulfate to the aqueous solution prepared in step (1);

(4)把步骤(1)、(2)和(3)所配制的水溶液注入容器中,通入氮气3~5分钟后,密闭容器; (4) Pour the aqueous solution prepared in steps (1), (2) and (3) into the container, and after 3 to 5 minutes of nitrogen gas, airtight the container;

(5)置于58±2 ℃的水浴中5 小时以上; (5) Place in a water bath at 58±2°C for more than 5 hours;

(6)将淡黄色粘稠状产物洗涤后,置于真空干燥箱干燥,得到聚丙烯酸钠。 (6) Wash the pale yellow viscous product and dry it in a vacuum oven to obtain sodium polyacrylate.

2、聚丙烯酰胺的制备 2. Preparation of polyacrylamide

(1)把300 g丙烯酰胺溶于质量分数为910 g水中,配制成水溶液; (1) Dissolve 300 g of acrylamide in water with a mass fraction of 910 g to prepare an aqueous solution;

(2)把5 g碳酸钠,加入步骤(1)配制的水溶液中; (2) Add 5 g of sodium carbonate to the aqueous solution prepared in step (1);

(3)把0.5 g碳酰二胺脲和0.5 g过硫酸铵,加入步骤(1)配制的水溶液中; (3) Add 0.5 g carbodiamide and 0.5 g ammonium persulfate to the aqueous solution prepared in step (1);

(4)把步骤(1)、(2)和(3)所配制的水溶液注入容器中,通入氮气5分钟后,密闭容器; (4) Pour the aqueous solution prepared in steps (1), (2) and (3) into the container, and after passing nitrogen gas for 5 minutes, seal the container;

(5)置于20±2 ℃的水浴中8 小时以上; (5) Place in a water bath at 20±2°C for more than 8 hours;

(6)将透明粘稠状产物洗涤后,置于真空干燥箱干燥,得到分子量为大于1×107的聚丙烯酰胺。 (6) Wash the transparent viscous product and dry it in a vacuum oven to obtain polyacrylamide with a molecular weight greater than 1×10 7 .

3、压裂液的配制 3. Preparation of fracturing fluid

(1)把10 g乙二醇加入890 g水中; (1) Add 10 g of ethylene glycol to 890 g of water;

(2)加入50 g聚丙烯酸钠、 50 g聚丙烯酰胺和 30 g十六烷基二羟乙基甜菜碱,搅拌直至形成均匀透明的溶液; (2) Add 50 g sodium polyacrylate, 50 g polyacrylamide and 30 g hexadecyl dihydroxyethyl betaine, and stir until a uniform and transparent solution is formed;

(3)加入质量分数20 g氯化钠和 1 g羟基苯甲酸钠,搅拌均匀,得到压裂液。 (3) Add 20 g of sodium chloride and 1 g of sodium hydroxybenzoate in mass fraction, and stir evenly to obtain fracturing fluid.

实施例二Embodiment two

1、聚丙烯酸钠的制备; 1. Preparation of sodium polyacrylate;

(1)把500 g的丙烯酸钠溶于质量分数为1000 g的水中,配制成水溶液; (1) Dissolve 500 g of sodium acrylate in water with a mass fraction of 1000 g to prepare an aqueous solution;

(2)把7 g的碳酸钠,加入步骤(1)配制的水溶液中; (2) Add 7 g of sodium carbonate to the aqueous solution prepared in step (1);

(3)把质量分数为2.5 g的十二硫醇和2.5 g 的过硫酸钾,加入步骤(1)配制的水溶液中; (3) Add 2.5 g of dodecanethiol and 2.5 g of potassium persulfate to the aqueous solution prepared in step (1);

(4)把步骤(1)、(2)和(3)所配制的水溶液注入容器中,通入氮气3~5分钟后,密闭容器; (4) Pour the aqueous solution prepared in steps (1), (2) and (3) into the container, and after 3 to 5 minutes of nitrogen gas, airtight the container;

(5)置于58±2 ℃的水浴中5 小时以上; (5) Place in a water bath at 58±2°C for more than 5 hours;

(6)将淡黄色粘稠状产物洗涤后,置于真空干燥箱干燥,得到聚丙烯酸钠。 (6) Wash the pale yellow viscous product and dry it in a vacuum oven to obtain sodium polyacrylate.

2、聚丙烯酰胺的制备; 2. Preparation of polyacrylamide;

(1)把500 g丙烯酰胺溶于质量分数为1500 g水中,配制成水溶液; (1) Dissolve 500 g of acrylamide in water with a mass fraction of 1500 g to prepare an aqueous solution;

(2)把8.5 g碳酸钠,加入步骤(1)配制的水溶液中; (2) Add 8.5 g of sodium carbonate to the aqueous solution prepared in step (1);

(3)把0.8 g碳酰二胺脲和0.8 g过硫酸铵,加入步骤(1)配制的水溶液中; (3) Add 0.8 g carbodiamide and 0.8 g ammonium persulfate to the aqueous solution prepared in step (1);

(4)把步骤(1)、(2)和(3)所配制的水溶液注入容器中,通入氮气5分钟后,密闭容器; (4) Pour the aqueous solution prepared in steps (1), (2) and (3) into the container, and after passing nitrogen gas for 5 minutes, seal the container;

(5)置于20±2 ℃的水浴中8 小时以上; (5) Place in a water bath at 20±2°C for more than 8 hours;

(6)将透明粘稠状产物洗涤后,置于真空干燥箱干燥,得到分子量为大于1×107的聚丙烯酰胺。 (6) Wash the transparent viscous product and dry it in a vacuum oven to obtain polyacrylamide with a molecular weight greater than 1×10 7 .

3、压裂液的配制; 3. Preparation of fracturing fluid;

(1)把5 g乙二醇加入445 g水中; (1) Add 5 g of ethylene glycol to 445 g of water;

(2)加入25 g聚丙烯酸钠、 25 g聚丙烯酰胺和 15 g十六烷基二羟乙基甜菜碱,搅拌直至形成均匀透明的溶液; (2) Add 25 g sodium polyacrylate, 25 g polyacrylamide and 15 g hexadecyl dihydroxyethyl betaine, and stir until a uniform and transparent solution is formed;

(3)加入质量分数10 g氯化钠和 0.5 g羟基苯甲酸钠,搅拌均匀,得到压裂液。 (3) Add mass fractions of 10 g sodium chloride and 0.5 g sodium hydroxybenzoate, and stir evenly to obtain fracturing fluid.

实施例三Embodiment three

1、聚丙烯酸钠的制备 1. Preparation of sodium polyacrylate

(1)把1000 g的丙烯酸钠溶于质量分数为2000 g的水中,配制成水溶液; (1) Dissolve 1000 g of sodium acrylate in water with a mass fraction of 2000 g to prepare an aqueous solution;

(2)把15g的碳酸钠,加入步骤(1)配制的水溶液中; (2) Add 15g of sodium carbonate to the aqueous solution prepared in step (1);

(3)把质量分数为5 g的十二硫醇和5 g 的过硫酸钾,加入步骤(1)配制的水溶液中; (3) Add 5 g of dodecanethiol and 5 g of potassium persulfate to the aqueous solution prepared in step (1);

(4)把步骤(1)、(2)和(3)所配制的水溶液注入容器中,通入氮气3~5分钟后,密闭容器; (4) Pour the aqueous solution prepared in steps (1), (2) and (3) into the container, and after 3 to 5 minutes of nitrogen gas, airtight the container;

(5)置于58±2 ℃的水浴中5 小时以上; (5) Place in a water bath at 58±2°C for more than 5 hours;

(6)将淡黄色粘稠状产物洗涤后,置于真空干燥箱干燥,得到聚丙烯酸钠。 (6) Wash the pale yellow viscous product and dry it in a vacuum oven to obtain sodium polyacrylate.

2、聚丙烯酰胺的制备 2. Preparation of polyacrylamide

(1)把1000 g丙烯酰胺溶于质量分数为3000 g水中,配制成水溶液; (1) Dissolve 1000 g of acrylamide in water with a mass fraction of 3000 g to prepare an aqueous solution;

(2)把17 g碳酸钠,加入步骤(1)配制的水溶液中; (2) Add 17 g of sodium carbonate to the aqueous solution prepared in step (1);

(3)把1.5 g碳酰二胺脲和1.5 g过硫酸铵,加入步骤(1)配制的水溶液中; (3) Add 1.5 g carbodiamide and 1.5 g ammonium persulfate to the aqueous solution prepared in step (1);

(4)把步骤(1)、(2)和(3)所配制的水溶液注入容器中,通入氮气5分钟后,密闭容器; (4) Pour the aqueous solution prepared in steps (1), (2) and (3) into the container, and after passing nitrogen gas for 5 minutes, seal the container;

(5)置于20±2 ℃的水浴中8 小时以上; (5) Place in a water bath at 20±2°C for more than 8 hours;

(6)将透明粘稠状产物洗涤后,置于真空干燥箱干燥,得到分子量为大于1×107的聚丙烯酰胺。 (6) Wash the transparent viscous product and dry it in a vacuum oven to obtain polyacrylamide with a molecular weight greater than 1×10 7 .

3、压裂液的配制 3. Preparation of fracturing fluid

(1)把20 g乙二醇加入1780 g水中; (1) Add 20 g of ethylene glycol to 1780 g of water;

(2)加入50 g聚丙烯酸钠、 50 g聚丙烯酰胺和 30 g十六烷基二羟乙基甜菜碱,搅拌直至形成均匀透明的溶液; (2) Add 50 g sodium polyacrylate, 50 g polyacrylamide and 30 g hexadecyl dihydroxyethyl betaine, and stir until a uniform and transparent solution is formed;

(3)加入质量分数20 g氯化钠和 1.0 g羟基苯甲酸钠,搅拌均匀,得到压裂液。 (3) Add 20 g of sodium chloride and 1.0 g of sodium hydroxybenzoate in mass fraction, and stir evenly to obtain fracturing fluid.

Claims (4)

1.一种中高温压裂液,其特征在于:分子量1000~2000的聚丙烯酸钠的质量分数5%,分子量大于1×107的聚丙烯酰胺的质量分数5%,十六烷基二羟乙基甜菜碱的质量分数3%,氯化钠的质量分数2%,乙二醇的质量分数1%,羟基苯甲酸钠的质量分数0.1%,余量为水。 1. A medium-high temperature fracturing fluid, characterized in that: 5% by mass fraction of sodium polyacrylate with a molecular weight of 1000-2000, 5% by mass fraction of polyacrylamide with a molecular weight greater than 1× 107 , cetyl dihydroxy The mass fraction of ethyl betaine is 3%, the mass fraction of sodium chloride is 2%, the mass fraction of ethylene glycol is 1%, the mass fraction of sodium hydroxybenzoate is 0.1%, and the balance is water. 2.根据权利要求1所述的一种中高温压裂液,其特征在于:所述分子量1000~2000的聚丙烯酸钠的合成方法步骤为: 2. A kind of medium-high temperature fracturing fluid according to claim 1, characterized in that: the synthesis method steps of the sodium polyacrylate with molecular weight 1000~2000 are: (1)把质量分数为30%的丙烯酸钠溶于质量分数为60%的水中,配制成水溶液; (1) Dissolve sodium acrylate with a mass fraction of 30% in water with a mass fraction of 60% to prepare an aqueous solution; (2)把质量分数为4%的碳酸钠,加入步骤(1)配制的水溶液中; (2) adding mass fraction of 4% sodium carbonate to the aqueous solution prepared in step (1); (3)把质量分数为1.5%的十二硫醇和1.5%的过硫酸钾,加入步骤(1)配制的水溶液中; (3) adding 1.5% dodecanethiol and 1.5% potassium persulfate to the aqueous solution prepared in step (1) with a mass fraction; (4)把步骤(1)、(2)和(3)所配制的水溶液注入容器中,通入氮气3~5分钟后,密闭容器; (4) Pour the aqueous solution prepared in steps (1), (2) and (3) into the container, and after 3 to 5 minutes of nitrogen gas, airtight the container; (5)置于58±2 ℃的水浴中5 小时以上; (5) Place in a water bath at 58±2°C for more than 5 hours; (6)将淡黄色粘稠状产物洗涤后,置于真空干燥箱干燥,得到分子量为1000~2000的聚丙烯酸钠。 (6) Wash the pale yellow viscous product and dry it in a vacuum oven to obtain sodium polyacrylate with a molecular weight of 1000-2000. 3.根据权利要求1所述的一种中高温压裂液,其特征在于:所述分子量大于1×107的聚丙烯酰胺的合成方法步骤为: 3. A medium-high temperature fracturing fluid according to claim 1, characterized in that: the steps of the synthesis method of the polyacrylamide having a molecular weight greater than 1×10 7 are: (1)把质量分数为24%的丙烯酰胺溶于质量分数为73%的水中,配制成水溶液; (1) Dissolve acrylamide with a mass fraction of 24% in water with a mass fraction of 73% to prepare an aqueous solution; (2)把质量分数为2.5%的碳酸钠,加入步骤(1)配制的水溶液中; (2) adding mass fraction of 2.5% sodium carbonate to the aqueous solution prepared in step (1); (3)把质量分数为0.25%的碳酰二胺脲和0.25%的过硫酸铵,加入步骤(1)配制的水溶液中; (3) Add carbodiamide urea and 0.25% ammonium persulfate with a mass fraction of 0.25% to the aqueous solution prepared in step (1); (4)把步骤(1)、(2)和(3)所配制的水溶液注入容器中,通入氮气5分钟后,密闭容器; (4) Pour the aqueous solution prepared in steps (1), (2) and (3) into the container, and after passing nitrogen gas for 5 minutes, seal the container; (5)置于20±2 ℃的水浴中8 小时以上; (5) Place in a water bath at 20±2°C for more than 8 hours; (6)将透明粘稠状产物洗涤后,置于真空干燥箱干燥,得到分子量为大于1000万的聚丙烯酰胺。 (6) Wash the transparent viscous product and dry it in a vacuum oven to obtain polyacrylamide with a molecular weight greater than 10 million. 4.一种如权利要求1所述中高温压裂液的制备方法,其特征在于:首先把乙二醇加入水中,再加入聚丙烯酸钠、聚丙烯酰胺和十六烷基二羟乙基甜菜碱,搅拌直至形成均匀透明的溶液,最后加入氯化钠和羟基苯甲酸钠搅拌均匀后得到。 4. A preparation method of medium-high temperature fracturing fluid as claimed in claim 1, characterized in that: first ethylene glycol is added to water, then sodium polyacrylate, polyacrylamide and cetyl dihydroxyethyl beet are added Alkali, stir until a uniform and transparent solution is formed, and finally add sodium chloride and sodium hydroxybenzoate and stir evenly to obtain.
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Application publication date: 20141119