CN117402602A - Integrated fracturing fluid and preparation method thereof - Google Patents

Integrated fracturing fluid and preparation method thereof Download PDF

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CN117402602A
CN117402602A CN202210793627.1A CN202210793627A CN117402602A CN 117402602 A CN117402602 A CN 117402602A CN 202210793627 A CN202210793627 A CN 202210793627A CN 117402602 A CN117402602 A CN 117402602A
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fracturing fluid
water
viscosity
integrated
fluorine
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熊颖
张亚东
张大椿
黄晨直
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Petrochina Co Ltd
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Petrochina Co Ltd
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Priority to CN202210793627.1A priority Critical patent/CN117402602A/en
Priority to PCT/CN2023/095431 priority patent/WO2024007750A1/en
Publication of CN117402602A publication Critical patent/CN117402602A/en
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Abstract

The invention provides an integrated fracturing fluid and a preparation method thereof. The fracturing fluid comprises the following components: 0.02-0.5% of resistance-reducing tackifier, 0.1-0.5% of nano emulsion, 0.02-0.1% of nonionic fluorocarbon surfactant, 0.003-0.05% of bactericide, 0-0.5% of viscosity regulator, 0-0.5% of clay stabilizer, 0-0.1% of gel breaker, 0.05-0.2% of modifier, 0.1-0.5% of gas producer and the balance of water. The preparation method of the fracturing fluid comprises the following steps: adding a resistance-reducing tackifier into water, and adding a bactericide, a clay stabilizer, a modifier, a nano emulsion and a nonionic fluorocarbon surfactant; adding a viscosity regulator according to the viscosity requirement; then adding a gas generating agent and a gel breaker; or adding the gas generating agent and the gel breaker into a sand mixing tank to be mixed with the mixed liquid and the sand. The integrated fracturing fluid provided by the invention has low friction resistance, adjustable viscosity and high sand suspending performance under the same viscosity.

Description

Integrated fracturing fluid and preparation method thereof
Technical Field
The invention relates to an integrated fracturing fluid and a preparation method thereof, and belongs to the technical field of oilfield chemistry.
Background
Unconventional gas reservoirs such as shale oil gas, compact oil gas and the like have become key and hot spot fields for oil and gas exploration and development. At present, the volume fracturing mode is mainly adopted for the reconstruction operation of the unconventional oil and gas reservoirs, the required fracturing fluid is mainly slickwater and glue solution (linear glue, jelly glue or weak gel), more viscosity-adjustable slickwater fracturing fluid is adopted in the practical application process, the slickwater fracturing fluid is used as the general slickwater fracturing fluid at low viscosity, the linear gel fracturing fluid is used as the linear gel fracturing fluid at medium viscosity, and the weak gel or jelly glue fracturing fluid is used at high viscosity. The low-viscosity fracturing fluid has low friction, but poor sand suspending performance, and the high-viscosity fracturing fluid has good sand suspending performance, but higher friction. In addition, too high viscosity can cause the fracture to be simpler, and complex fracture network is difficult to form, and the final fracturing effect is affected. Therefore, an integrated fracturing fluid with good performance is an important point of volume fracturing fluid research.
CN110003877a discloses a clean viscosity-variable slick water with high mineralization resistance, the cross-linking agent is an organoboron/zirconium composite cross-linking agent, and the viscosity-variable friction reducer is cross-linked to increase the viscosity.
CN111763511a discloses a preparation method and a fluid preparation method of an integrated self-crosslinking thickener modified polymer for fracturing, which can be used for preparing slickwater and sand suspension fracturing fluid. The thickening agent is polymer emulsion polymerized by reverse phase emulsion, the addition amount of the thickening agent in slickwater is 0.06-0.12%, and the addition amount of the thickening agent in the suspended sand fracturing fluid is 1-2%, and the viscosity change of the slickwater fracturing fluid is realized by the change of the concentration of the polymer.
CN113025302a discloses an integrated self-crosslinking fracturing fluid, which uses a self-crosslinking emulsion fracturing fluid thickener, and uses water solutions with different mass fractions as fracturing fluid, namely 0.05-0.4% of thickener solution is used as slick water fracturing fluid, 0.4-2.0% of thickener solution is used as sand suspending fracturing fluid, and the switching between slick water and sand suspending fluid is realized through the adjustment of the addition amount.
CN112375557a discloses an alcohol-soluble slick water for fracturing, which consists of 20.0-60.0% of polyacrylamide polymer, 0.5-4.0% of nano particles, 0.1-3% of surfactant and organic alcohol.
CN112126419a discloses a sand suspension capable of being continuously prepared, which comprises 1-10 parts of thickening agent, 1-5 parts of cross-linking agent, 900-1000 parts of water and 20-60 parts of propping agent.
CN111635749a discloses a slick water system with both drag reduction and suspended sand, which consists of 0.02-0.3 wt% of instant association polymer drag reducer, 0.01-0.1 wt% of nonionic surfactant and/or anionic surfactant, 0.1-2 wt% of clay stabilizer and water, and the viscosity is adjustable within 20 mpa.s.
CN111647106a discloses viscoelastic polymer emulsion type slick water and sand suspension, and adopts inverse emulsion polymerization to prepare nano-scale viscoelastic polymer emulsion, which overcomes the defect of low copolymerization rate of the existing associative monomer in the inverse emulsion polymerization process.
Under the same fracturing displacement condition, the prior art for improving sand suspension performance is mainly realized by means of thickening of fracturing fluid: the polymer viscosity-increasing agent or thickener is thickened by increasing the concentration of the polymer viscosity-increasing agent or is thickened by crosslinking with a crosslinking agent under a certain polymer concentration or is thickened by intramolecular intermolecular association after the concentration of the hydrophobic association polymer type viscosity-increasing agent or thickener reaches a certain degree.
However, these prior arts have at least the following problems: the concentration of the friction reducing agent or the thickening agent and the concentration of the matched cross-linking agent are required to be greatly improved to improve the sand suspension performance, and the cost of the fracturing fluid is high; under the same condition, the higher the viscosity of the fracturing fluid is, the larger the friction resistance is, so that the friction resistance of the prior art under the high-viscosity condition is high, and the construction pump pressure is increased; in order to improve sand suspension performance, the viscosity of the fracturing fluid is greatly improved, and the too high viscosity of the fracturing fluid can lead to single cracks generated by fracturing, so that the complexity of a net formed by fracturing is low, and the volume fracturing effect is influenced.
Disclosure of Invention
In order to solve the technical problems, the invention aims to provide an integrated fracturing fluid and a preparation method thereof. The integrated fracturing fluid provided by the invention has the advantages of low friction resistance, adjustable viscosity, high sand suspension performance under the same viscosity condition and the like.
In order to achieve the above purpose, the first aspect of the present invention provides an integrated fracturing fluid, which comprises the following components in percentage by mass: 0.02-0.5% of resistance-reducing tackifier, 0.1-0.5% of nano emulsion, 0.02-0.1% of first nonionic fluorocarbon surfactant, 0.003-0.05% of bactericide, 0-0.5% of viscosity regulator, 0-0.5% of clay stabilizer, 0-0.1% of gel breaker, 0.05-0.2% of modifier, 0.1-1% of gas producer and the balance of water.
According to a specific embodiment of the present invention, preferably, when the integrated fracturing fluid contains a viscosity modifier, the content of the viscosity modifier may be generally controlled to be 0.1 to 0.5% based on 100% of the total mass of the integrated fracturing fluid.
According to a specific embodiment of the present invention, when the integrated fracturing fluid contains a breaker, the content of the breaker may be generally controlled to be 0.02-0.1% based on 100% of the total mass of the integrated fracturing fluid.
According to a specific embodiment of the present invention, preferably, when the integrated fracturing fluid contains a clay stabilizer, the content of the clay stabilizer may be generally controlled to be 0.01-0.5% based on 100% of the total mass of the integrated fracturing fluid.
According to a specific embodiment of the present invention, preferably, when the integrated fracturing fluid is a low-viscosity fracturing fluid (kinematic viscosity. Ltoreq.5 mm 2 And/s), the composition comprises the following components in percentage by mass: 0.02% -0.05% of resistance-reducing tackifier, 0.1% -0.5% of nano emulsion, 0.02% -0.1% of first nonionic fluorocarbon surfactant, 0.003% -0.05% of bactericide, 0-0.5% of clay stabilizer, 0.05% -0.2% of modifier, 0.1% -0.5% of gas generating agent and the balance of water. More preferably, when the integrated fracturing fluid is a low viscosity fracturing fluid, it comprises the following components in mass percent: 0.03 to 0.05 percent of resistance-reducing tackifier, 0.1 to 0.4 percent of nano emulsion, 0.02 to 0.08 percent of first nonionic fluorocarbon surfactant, 0.005 to 0.02 percent of bactericide, 0.1 to 0.3 percent of clay stabilizer, 0.08 to 0.15 percent of modifier, 0.2 to 0.4 percent of gas generating agent and the balance of water.
According to a specific embodiment of the present invention, preferably, when the integrated fracturing fluid is a medium viscosity fracturing fluid (apparent viscosity is 12 to 30mpa·s), it comprises the following components in mass percent: 0.2 to 0.5 percent of resistance-reducing tackifier, 0.1 to 0.5 percent of nano emulsion, 0.02 to 0.1 percent of first nonionic fluorocarbon surfactant, 0.003 to 0.05 percent of bactericide, 0 to 0.5 percent of clay stabilizer, 0.02 to 0.1 percent of gel breaker, 0.05 to 0.2 percent of modifier, 0.1 to 0.5 percent of gas producer and the balance of water. More preferably, when the integrated fracturing fluid is a medium viscosity fracturing fluid, it comprises the following components in mass percent: 0.2 to 0.4 percent of resistance-reducing tackifier, 0.1 to 0.4 percent of nano emulsion, 0.02 to 0.08 percent of first nonionic fluorocarbon surfactant, 0.005 to 0.02 percent of bactericide, 0.1 to 0.3 percent of clay stabilizer, 0.02 to 0.08 percent of gel breaker, 0.08 to 0.15 percent of modifier, 0.2 to 0.4 percent of gas producer and the balance of water.
According to a specific embodiment of the present invention, preferably, when the integrated fracturing fluid is a high-viscosity fracturing fluid (apparent viscosity is 50-200mpa·s), it comprises the following components in mass percent: 0.3 to 0.5 percent of resistance-reducing tackifier, 0.1 to 0.5 percent of nano emulsion, 0.02 to 0.1 percent of first nonionic fluorocarbon surfactant, 0.003 to 0.05 percent of bactericide, 0.1 to 0.5 percent of viscosity regulator, 0 to 0.5 percent of clay stabilizer, 0.06 to 0.1 percent of gel breaker, 0.05 to 0.2 percent of modifier, 0.1 to 0.5 percent of gas producer and the balance of water. More preferably, when the integrated fracturing fluid is a high viscosity fracturing fluid, it comprises the following components in mass percent: 0.3 to 0.5 percent of resistance-reducing tackifier, 0.1 to 0.4 percent of nano emulsion, 0.02 to 0.08 percent of first nonionic fluorocarbon surfactant, 0.005 to 0.02 percent of bactericide, 0.25 to 0.45 percent of viscosity regulator, 0.1 to 0.3 percent of clay stabilizer, 0.06 to 0.1 percent of gel breaker, 0.08 to 0.15 percent of modifier, 0.2 to 0.4 percent of gas producer and the balance of water.
In the above integrated fracturing fluid, preferably, the resistance-reducing tackifier is a mixture of hydrolyzed polyacrylamide and/or its derivative and non-hydrolyzed polyacrylamide and/or its derivative. More preferably, the mass ratio of the hydrolyzed polyacrylamide and/or derivative thereof to the non-hydrolyzed polyacrylamide and/or derivative thereof is (10-15): 1.
in the above-mentioned integrated fracturing fluid, preferably, in the resistance-reducing tackifier, the viscosity average molecular weight of the hydrolyzed polyacrylamide and/or its derivative is 500 to 1500 tens of thousands, and the degree of hydrolysis is 20 to 30%; the viscosity average molecular weight of the non-hydrolytic polyacrylamide and/or the derivative thereof is 500 ten thousand to 1500 ten thousand.
The anti-drag tackifier adopted by the fracturing fluid is a mixture of hydrolyzed polyacrylamide and/or a derivative thereof and non-hydrolyzed polyacrylamide and/or a derivative thereof, and the mass ratio of the hydrolyzed polyacrylamide and/or the derivative thereof is (10-15): 1, the viscosity average molecular weight of the two is 500 ten thousand to 1500 ten thousand. The hydrolyzed polyacrylamide contains a large number of carboxyl groups, and the hydrolyzed polyacrylamide and the central ion of the cross-linking agent (namely the viscosity regulator) have cross-linking effect under a certain concentration, so that a net structure is formed, the viscosity of the fracturing fluid is greatly improved, and the sand suspension performance is improved by virtue of high viscosity. Compared with the use amount concentration of the hydrolyzed polyacrylamide, the non-hydrolyzed polyacrylamide has low dosage concentration, does not generate crosslinking reaction with the central ion of the crosslinking agent (namely the viscosity regulator) under a certain concentration, and still keeps a non-crosslinked linear high polymer state, and is stretched in the fracturing fluid, so that the fracturing fluid still has higher resistance reduction under the condition of high viscosity. Therefore, the invention overcomes the contradiction between low friction resistance and high sand suspension of the fracturing fluid by combining the hydrolyzed polyacrylamide and/or the derivative thereof with the non-hydrolyzed polyacrylamide and/or the derivative thereof in a specific proportion.
In the above integrated fracturing fluid, preferably, the nanoemulsion is a nanoemulsion having an average particle diameter of 150nm or less.
In the above integrated fracturing fluid, preferably, the total mass of the nanoemulsion is 100%, which comprises the following components: 10% -20% of fluorine-containing silicone oil, 5% -10% of gemini fluorocarbon surfactant, 15% -25% of second nonionic fluorocarbon surfactant, 5% -10% of nano silicon dioxide, 1% -10% of lower alcohol and the balance of water.
In the above-described integrated fracturing fluid, preferably, in the nanoemulsion, the fluorine-containing silicone oil includes one or a combination of several of hydroxyl fluorosilicone oil, vinyl fluorosilicone oil, methyl fluorosilicone oil, polyether fluorosilicone oil and the like.
In the above integrated fracturing fluid, preferably, in the nanoemulsion, the structural general formula of the gemini fluorocarbon surfactant is: c (C) n F 2n+1 N + (CH 3 ) 2 -CH 2 CH 2 CH 2 CH 2 -(CH 3 ) 2 N + C n F 2n+1 Wherein n is 2-4.
More preferably, the gemini fluorocarbon surfactant is prepared by: adding 1-3 parts of fluorine-containing bromoalkane into a solvent at 20-40 ℃ in parts by weight, stirring and mixing uniformly (the stirring rotating speed is preferably 100-300 rpm), then dripping 0.5-1.5 parts of tetramethylbutanediamine (the dripping acceleration is preferably uniformly dripping in 10-20 min), carrying out quaternization reaction (the stirring rotating speed is preferably 100-300 rpm) under stirring, and reacting for 0.5-2h to obtain precipitate, namely the gemini fluorocarbon surfactant. Among them, it is particularly preferable that the fluorine-containing bromoalkane includes one or a combination of several of heptafluoro-2-bromopropane, pentafluorobromide, 1-nonafluorobutyl bromide and the like. The solvent may include acetone or the like, and may be used in an amount of 7 to 10 parts by weight. In addition, the precipitate obtained after the reaction may be subjected to conventional filtration, washing and the like, and the present invention is not particularly limited to these conventional operations.
In the above-mentioned integrated fracturing fluid, preferably, in the nanoemulsion, the second nonionic fluorocarbon surfactant includes one or a combination of several of polyoxyethylene ether of fluorine-containing fatty alcohol, polyoxyethylene ether of fluorine-containing phenol, polyoxyethylene ether of fluorine-containing alkyl sulfonyl alcohol amine, polyoxyethylene ester of fluorine-containing carboxylic acid, polyoxyethylene ether of fluorine-containing thiol, and the like. More specifically, the second nonionic fluorocarbon surfactant includes, but is not limited to: one or a combination of several of a nonionic fluorocarbon surfactant capsule FS-30 of dupont, a nonionic fluorocarbon surfactant FCF-204 of Guangzhou Shunchun new materials science and technology limited, a nonionic fluorocarbon surfactant FC4430 of 3M, a nonionic fluorocarbon surfactant FC4432 of 3M, a nonionic fluorocarbon surfactant KHD011 of Sichuan macro-da group, a nonionic fluorocarbon surfactant KX-109 of Guangzhou Kang Lunxi fluorosilicon materials limited, a nonionic fluorocarbon surfactant capsule FS-3100 of dupont, a nonionic fluorocarbon surfactant AF4018-Y of Anhui gold chemical limited, and the like.
In the above integrated fracturing fluid, preferably, in the nanoemulsion, the particle size of the nano silica is 15-50nm.
In the above-described integrated fracturing fluid, preferably, in the nanoemulsion, the lower alcohol includes one or a combination of several of methanol, ethanol, propanol, butanol, and the like.
In the above integrated fracturing fluid, preferably, the nanoemulsion is prepared by the following steps: according to the content of each component in the nano emulsion, adding a gemini fluorocarbon surfactant and a nonionic fluorocarbon surfactant into water at the temperature of 10-40 ℃ and the stirring speed of 120-600rpm, and then stirring for 10-30min; adding lower alcohol, and stirring for 10-30min; adding nano silicon dioxide, and continuing stirring for 10-30min; dripping fluorine-containing silicone oil, and continuously stirring for 30-60min; finally, ultrasonic treatment is carried out for 20-40min, and the nano emulsion is obtained. Wherein, more preferably, the frequency of the ultrasonic wave is 15-20 kilohertz. The dripping speed of the fluorine-containing silicone oil is preferably 30min, and the uniform dripping is finished.
The fracturing fluid adopts the nano emulsion with the average particle size of the liquid drops less than or equal to 150nm, can enter into micro cracks of a stratum, and plays roles in gas-liquid replacement and improving seepage and absorption of the stratum.
In the above integrated fracturing fluid, preferably, the first nonionic fluorocarbon surfactant includes one or a combination of several of polyoxyethylene ether of fluorine-containing fatty alcohol, polyoxyethylene ether of fluorine-containing phenol, polyoxyethylene ether of fluorine-containing alkyl sulfonyl alcohol amine, polyoxyethylene ester of fluorine-containing carboxylic acid, polyoxyethylene ether of fluorine-containing thiol, and the like. More specifically, the first nonionic fluorocarbon surfactant includes, but is not limited to: one or a combination of several of a nonionic fluorocarbon surfactant capsule FS-30 of dupont, a nonionic fluorocarbon surfactant FCF-204 of Guangzhou Shunchun new materials science and technology limited, a nonionic fluorocarbon surfactant FC4430 of 3M, a nonionic fluorocarbon surfactant FC4432 of 3M, a nonionic fluorocarbon surfactant KHD011 of Sichuan macro-da group, a nonionic fluorocarbon surfactant KX-109 of Guangzhou Kang Lunxi fluorosilicon materials limited, a nonionic fluorocarbon surfactant capsule FS-3100 of dupont, a nonionic fluorocarbon surfactant AF4018-Y of Anhui gold chemical limited, and the like. The first nonionic fluorocarbon surfactant can cooperate with the nanoemulsion disclosed by the invention to reduce the surface tension of the fracturing fluid and reduce the capillary resistance of the fracturing fluid flowing in the micro-cracks of the stratum.
In the above-described integrated fracturing fluid, preferably, the bactericide includes one or a combination of several of aldehyde bactericides, quaternary ammonium salt bactericides, isothiazolinone bactericides and the like.
In the above-mentioned integrated fracturing fluid, preferably, the aldehyde sterilizing agent includes one or a combination of several of glutaraldehyde, formaldehyde, acrolein and the like.
In the above-mentioned integrated fracturing fluid, preferably, the quaternary ammonium salt bactericide includes one or a combination of several of tetradecyldimethylbenzyl ammonium chloride, dodecyl trimethyl ammonium chloride, dodecyl dimethylbenzyl ammonium bromide and the like.
In the above-described integrated fracturing fluid, preferably, the isothiazolinone bactericide includes methyl isothiazolinone, methyl chloroisothiazolinone, or the like.
The bactericide adopted by the fracturing fluid can kill bacteria in the fracturing fluid and inhibit bacterial growth, so that the problems of corrosion caused by bacterial growth, micro-crack blockage caused by bacterial metabolites and the like are avoided.
In the above-described integrated fracturing fluid, preferably, the viscosity modifier includes one or a combination of several of a water-soluble zirconium salt, a water-soluble titanium salt, a water-soluble chromium salt, a water-soluble aluminum salt, and the like. More preferably, the viscosity modifier comprises: and one or a combination of a plurality of water-soluble organic zirconium salt, water-soluble organic titanium salt, water-soluble organic chromium salt, water-soluble organic aluminum salt and the like which are obtained by complexing water-soluble zirconium salt, water-soluble titanium salt, water-soluble chromium salt, water-soluble aluminum salt and the like with polyhydroxy alcohol respectively. The viscosity regulator adopted by the invention can be crosslinked with the hydrolyzed polyacrylamide and/or the derivative thereof in the resistance-reducing tackifier to greatly improve the viscosity of the fracturing fluid.
In the above integrated fracturing fluid, preferably, the water-soluble organic zirconium salt includes a complex obtained by a complexation reaction of zirconium oxychloride with one or more of sorbitol, glycerol, ethylene glycol, 1, 2-propanediol, 1, 4-butanediol, diethylene glycol, triethylene glycol, and the like. More specifically, in the complexing reaction, the dosage mass ratio of the zirconium oxychloride to the polyhydroxy alcohol can be (5-20): (80-95), the complexing reaction temperature can be 50-90 ℃, and the reaction time can be 1-6h.
In the above-mentioned integrated fracturing fluid, preferably, the water-soluble organic titanium salt includes one or a combination of several of diisopropyl di (triethanolamine) titanate, tetraisopropyl orthotitanate, diisopropyl orthotitanate and diisopropyl orthotitanate; or a complex obtained by a complex reaction of one or more of diisopropyl di (triethanolamine) titanate, tetraisopropyl orthotitanate, diisopropyl orthotitanate, and diisopropyl orthotitanate with one or more of sorbitol, glycerol, ethylene glycol, 1, 2-propylene glycol, 1, 4-butanediol, diethylene glycol, triethylene glycol, etc. More specifically, in the complexing reaction, the mass ratio of the amount of one or more of diisopropyl di (triethanolamine) titanate, tetraisopropyl orthotitanate, diisopropyl orthotitanate and the like to the polyhydroxy alcohol may be (5-20): 80-95, the complexing reaction temperature may be 50-90 ℃, and the reaction time may be 1-6 hours.
In the above-mentioned integrated fracturing fluid, preferably, the water-soluble organic chromium salt includes a complex obtained by a complex reaction of one or a combination of several of chromium lactate, chromium acetate, chromium chloride, chromium sulfate and the like and one or a combination of several of sorbitol, glycerol, ethylene glycol, 1, 2-propanediol, 1, 4-butanediol, diethylene glycol, triethylene glycol and the like. More specifically, in the complexation reaction, the mass ratio of one or more of chromium lactate, chromium acetate, chromium chloride, chromium sulfate and the like to the amount of polyhydroxy alcohol may be (10-20): (80-90), the complexation reaction temperature may be 50-90 ℃, and the reaction time may be 1-3 hours.
In the above-mentioned integrated fracturing fluid, preferably, the water-soluble organic aluminum salt includes a complex obtained by complexation reaction of one or more of potassium aluminum sulfate dodecahydrate, aluminum sulfate, aluminum lactate, aluminum acetate, aluminum chloride, and the like, and one or more of sorbitol, glycerol, ethylene glycol, 1, 2-propylene glycol, 1, 4-butanediol, diethylene glycol, triethylene glycol, and the like. More specifically, in the complexation reaction, the mass ratio of one or more of aluminum potassium sulfate dodecahydrate, aluminum sulfate, aluminum lactate, aluminum acetate, aluminum chloride and the like to the amount of polyhydroxy alcohol may be (15-25): (75-85), the complexation reaction temperature may be 50-90 ℃, and the reaction time may be 1-3 hours.
In the above-described integrated fracturing fluid, preferably, the clay stabilizer includes one or a combination of several of tetramethyl ammonium chloride, potassium chloride, polyquaternium and the like.
In the above integrated fracturing fluid, preferably, the breaker includes one or a combination of several of ammonium persulfate, sodium persulfate, potassium persulfate, and the like. The gel breaker adopted by the invention can lead the gel produced by crosslinking the resistance-reducing tackifier and the viscosity-reducing tackifier with the viscosity regulator to break gel and degrade by oxidation, so as to reduce the adhesion and blockage damage of the high polymer to the stratum.
In the above integrated fracturing fluid, preferably, the modifier includes a silane modifier. More preferably, the silane modifier comprises one or a combination of a plurality of N-beta-aminoethyl-gamma-aminopropyl methyl dimethoxy silane, 3-aminopropyl triethoxy silane, N-beta-aminoethyl-gamma-aminopropyl trimethoxy silane and the like. The modifier adopted by the invention can be adsorbed on the surface of sand (i.e. ceramsite, quartz sand and the like) in the fracturing process, so that the surface of the sand is changed from hydrophilicity to oiliness to lipophobicity, thereby adsorbing dissolved gas in the fracturing fluid and/or gas generated by the gas generating agent, and surrounding the adsorbed gas on the surface of the sand, thereby suspending the sand in the fracturing fluid.
In the above-described integrated fracturing fluid, preferably, the gas generating agent includes effervescent tablet particles or the like. More preferably, the effervescent tablet particles are effervescent tablet particles with acid source of citric acid, alkali source of sodium bicarbonate and polyethylene glycol as coating. More preferably, the gas generating agent is prepared by the following steps: dissolving polyethylene glycol (preferably PEG-6000) in water (the temperature of the water can be 80-90 ℃) to form a sticky substance (the mass fraction of the polyethylene glycol in the sticky substance is 60-90%), and dividing the sticky substance into two parts (the mass ratio of the two parts of sticky substance can be 1:1-1:1.8); mixing citric acid and sodium bicarbonate with the two divided sticky substances (the mass ratio of the citric acid to the sticky substances can be 1:1-1:1.2, and the mass ratio of the sodium bicarbonate to the sticky substances can be 1:1-1:1.2), uniformly stirring, drying (the drying temperature can be 30-45 ℃), and pulverizing into powder to obtain acid source powder and alkali source powder respectively; adding polyethylene glycol (preferably PEG-800) into the acid source powder and the alkali source powder respectively (the adding amount of the polyethylene glycol in the step can be 3% -8% based on the total weight of the acid source powder and the polyethylene glycol as 100%, and the adding amount of the polyethylene glycol in the step can be 3% -8% based on the total weight of the alkali source powder and the polyethylene glycol as 100%), and uniformly mixing to obtain an acid source sticky substance and an alkali source sticky substance respectively; mixing the acid source sticky matter, the alkali source sticky matter and polyethylene glycol (PEG-6000 is preferable) according to the weight ratio of (1-2.5) to (0.1-0.2), tabletting after uniform mixing, granulating (and/or crushing) to obtain effervescent tablet particles, namely the gas generating agent.
The gas generating agent adopted by the invention can gradually dissolve polyethylene glycol coating in the fracturing fluid by means of stirring, so that an acid source and an alkali source are contacted in the fracturing fluid, carbon dioxide gas is released by acid-base reaction, and sand with the modifier adsorbed on the surface is adsorbed around the surface of the sand, so that the sand is suspended in the fracturing fluid.
The second aspect of the invention provides a preparation method of the integrated fracturing fluid, which comprises the following steps:
when indoor preparation is carried out:
s1, adding 0.02% -0.5% of resistance-reducing tackifier into water (the dosage of the water is calculated by adding the dosage of the other components to complement 100%) under the stirring condition of 60-200 rpm, and stirring and mixing uniformly;
s2, adding 0.003% -0.05% of bactericide, 0-0.5% of clay stabilizer, 0.05% -0.2% of modifier, 0.1% -0.5% of nano emulsion and 0.02% -0.1% of first nonionic fluorocarbon surfactant, and uniformly stirring and mixing to obtain a first mixed solution;
s3, adding 0-0.5% of viscosity regulator into the first mixed solution according to the viscosity requirement of the required fracturing fluid, and uniformly stirring and mixing to obtain a second mixed solution;
S4, adding 0.1-1% of a gas generating agent and 0-0.1% of a gel breaker into the second mixed solution, and uniformly stirring to obtain the integrated fracturing fluid (when the components of the fracturing fluid do not contain a viscosity regulator, the gas generating agent and the optional gel breaker are added into the first mixed solution);
when formulated in situ:
the preparation steps of S1-S3 are the same as those of indoor preparation, and the preparation steps of S4 are as follows: adding 0.1% -1% of gas generating agent and 0-0.1% of gel breaker into a sand mixing tank of a sand mixing vehicle, and uniformly mixing the gas generating agent, the gel breaker, the second mixed solution and sand in the sand mixing tank of the sand mixing vehicle.
In the preparation method of the present invention, when the integrated fracturing fluid of the present invention is a low-viscosity fracturing fluid, a medium-viscosity fracturing fluid, or a high-viscosity fracturing fluid, the amounts of the components are described above, and are not described herein, it will be understood by those skilled in the art that the fracturing fluid is configured according to the amounts of the components in the fracturing fluids of different viscosities and the preparation method described above.
The integrated fracturing fluid provided by the invention has the following advantages and beneficial effects:
under the same viscosity, the fracturing fluid provided by the invention has higher sand suspending performance than the conventional fracturing fluid, in particular to a low-viscosity slickwater fracturing fluid and a medium-viscosity linear gel fracturing fluid. Compared with the conventional fracturing fluid, the fracturing fluid provided by the invention has the advantages that the friction resistance is lower, the resistivity is improved by 2.1-11.2 percent, and the higher the viscosity is, the larger the amplitude of the resistivity improvement is. Meanwhile, the sand suspension performance of the fracturing fluid provided by the invention is superior to that of conventional fracturing fluid with the same viscosity, and particularly in the provided high-viscosity gel fracturing fluid, the sand suspension does not settle within 10min (in the conventional gel fracturing fluid with the same viscosity, the sand suspension settles for 10% within 10 min). Therefore, the integrated fracturing fluid provided by the invention has the advantages of low friction resistance, adjustable viscosity, high sand suspension performance under the same viscosity condition and the like.
Detailed Description
The technical solution of the present invention will be described in detail below for a clearer understanding of technical features, objects and advantageous effects of the present invention, but should not be construed as limiting the scope of the present invention.
Example 1
The embodiment provides an integrated fracturing fluid, which comprises the following components in percentage by mass: 0.03 percent of resistance-reducing tackifier, 0.1 percent of nano emulsion, 0.02 percent of nonionic fluorocarbon surfactant, 0.005 percent of bactericide, 0.2 percent of clay stabilizer, 0.08 percent of modifier, 0.2 percent of gas generating agent and the balance of water.
The viscosity-reducing tackifier is a mixture of polyacrylamide with viscosity-average molecular weight of 980 ten thousand and hydrolysis degree of 22 percent and non-hydrolyzed polyacrylamide with viscosity-average molecular weight of 1000 ten thousand +/-100 ten thousand, and the mass ratio of the two is 12:1.
The nanoemulsion is a nanoemulsion with an average particle size of 100 nm. Based on 100% of the total mass of the nanoemulsion, the nanoemulsion comprises: 15% methyl fluorosilicone oil (8012-300% of Guangzhou large-xi chemical raw material Co., ltd.) and 6% of gemini fluorocarbon surfactantAgent C 3 F 7 N + (CH 3 ) 2 -CH 2 CH 2 CH 2 CH 2 -(CH 3 ) 2 N + C 3 F 7 (self-made: 2 parts by weight of heptafluoro-2-bromopropane is added into 8 parts by weight of acetone at 25 ℃, uniformly mixed under stirring at 200rpm, 1 part by weight of tetramethylbutanediamine is added dropwise, uniformly and completely added for 10min, quaternization reaction is carried out under stirring at 200rpm, after reaction for 1h, the obtained precipitate is filtered and precipitated, and the obtained precipitate is the prepared binary fluorocarbon surfactant), 22% nonionic fluorocarbon surfactant (DuPont, capstone FS-30), 6% nano silicon dioxide with an average particle size of 20nm, 5% methanol and the balance of water.
The nanoemulsion is prepared by the following steps: according to the content of each component in the nano emulsion, adding water into a reaction kettle, and stirring at 35 ℃ and 300rpm to obtain the gemini fluorocarbon surfactant C 3 F 7 N + (CH 3 ) 2 -CH 2 CH 2 CH 2 CH 2 -(CH 3 ) 2 N + C 3 F 7 Adding the nonionic fluorocarbon surfactant into the reaction kettle, and stirring for 20min; adding methanol, and stirring for 20min; adding nano silicon dioxide, and continuing stirring for 20min; dripping methyl fluorosilicone oil at the speed of 30min after dripping, and continuously stirring for 40min; finally, ultrasonic treatment with the frequency of 20 kilohertz is adopted for 30 minutes to obtain the nano emulsion.
The nonionic fluorocarbon surfactant is Capstone FS-30 from DuPont.
The bactericide is glutaraldehyde.
The clay stabilizer is tetramethyl ammonium chloride.
The modifier is N-beta-aminoethyl-gamma-aminopropyl methyl dimethoxy silane (Wuhan Xin Wei Div chemical Co., ltd.).
The gas generating agent is effervescent tablet particles with citric acid as an acid source, sodium bicarbonate as an alkali source and polyethylene glycol as a coating. The preparation method comprises the following steps: dissolving polyethylene glycol (PEG-6000) in hot water at 80-90 ℃ to form a viscous substance, wherein the mass fraction of the polyethylene glycol (PEG-6000) in the viscous substance is 60-90%, and dividing the viscous substance into two parts (the mass ratio of the two parts of the viscous substance is 1:1); mixing citric acid and sodium bicarbonate with the two divided sticky matters respectively, wherein the mixing mass ratio of the citric acid to the sticky matters is 1:1-1:1.2, the mixing mass ratio of the sodium bicarbonate to the sticky matters is 1:1-1:1.2, uniformly stirring, drying at 30-45 ℃, and pulverizing into powder to obtain acid source powder and alkali source powder respectively; adding polyethylene glycol (PEG-800) into the acid source powder and the alkali source powder respectively, wherein the addition amount of the polyethylene glycol (PEG-800) is 3-8% based on 100% of the total weight of the acid source powder and the polyethylene glycol (PEG-800), and the addition amount of the polyethylene glycol (PEG-800) is 3-8% based on 100% of the total weight of the alkali source powder and the polyethylene glycol (PEG-800), and uniformly mixing to obtain an acid source sticky substance and an alkali source sticky substance respectively; mixing the acid source sticky matter, the alkali source sticky matter and polyethylene glycol (PEG-6000) according to the weight ratio of 2:1:0.1, tabletting, granulating and crushing after uniform mixing, thus obtaining effervescent tablet particles.
The preparation method of the integrated fracturing fluid of the embodiment comprises the following steps: slowly adding 0.03% of the resistance-reducing tackifier into water under the stirring condition of 100 revolutions per minute, and uniformly stirring and mixing; then sequentially adding 0.005% of the bactericide, 0.2% of the clay stabilizer, 0.08% of the modifier, 0.1% of the nanoemulsion and 0.02% of the nonionic fluorocarbon surfactant, and stirring and mixing uniformly; and finally, adding 0.2% of the gas generating agent, and uniformly stirring to obtain the integrated fracturing fluid.
Comparative examples 1 to 1
The nanoemulsion was removed from the fracturing fluid components of example 1, and the remaining components and contents were the same as those of the fracturing fluid preparation method, to obtain fracturing fluids of comparative examples 1-1.
Comparative examples 1 to 2
The nanoemulsion was replaced in the fracturing fluid composition of example 1, and the remaining components and contents were the same as those of the fracturing fluid preparation method, to obtain fracturing fluids of comparative examples 1 to 2.
The replaced nano emulsion does not contain gemini fluorocarbon surfactant C 3 F 7 N + (CH 3 ) 2 -CH 2 CH 2 CH 2 CH 2 -(CH 3 ) 2 N + C 3 F 7 The other components and contents were the same as in example 1. The preparation method comprises the following steps: according to the content of each component in the nano emulsion, adding water into a reaction kettle, adding a nonionic fluorocarbon surfactant (Capstone FS-30) into the reaction kettle at 35 ℃ and a stirring speed of 300rpm, and stirring for 20min; adding methanol, and stirring for 20min; adding nano silicon dioxide, and continuing stirring for 20min; and dripping methyl fluorosilicone oil at the speed of 30min after dripping, and continuously stirring for 40min to obtain the nano emulsion.
Conventional slick water fracturing fluid a:
based on 100% of the total mass of the conventional slick water fracturing fluid A, the slick water fracturing fluid A is prepared from 0.1% of polyacrylamide emulsion with 990 ten thousand viscosity average molecular weight and 25% of hydrolysis degree (Chengqiang Tech development Co., ltd., CT 1-20D), 0.1% of drainage aid (Chengqiang Tech development Co., ltd., CT 5-12), 0.005% of bactericide (Chengqiang Tech development Co., ltd., CT 10-4) and the balance of water.
Conventional slick water fracturing fluid B:
based on the total mass of the conventional slick water fracturing fluid B being 100%, the slick water fracturing fluid B is prepared from 0.03% of hydrophobic association polymer powder with viscosity average molecular weight of 880 ten thousand (Chengqiang Tech development Co., ltd., CT 1-20B), 0.1% of drainage aid (Chengqiang Tech development Co., ltd., CT 5-12), 0.005% of bactericide (Chengqiang Tech development Co., ltd., CT 10-4) and the balance of water.
The fracturing fluids prepared in the example 1 and the comparative examples 1-1 and 1-2 have low viscosity, and the main performances of the fracturing fluids are as follows from the line standard NB/T14003.1-2015, part 1 of shale gas fracturing fluid: the performance index of slick water and the evaluation method. The results of the main properties of the fracturing fluid are shown in table 1.
TABLE 1 fracturing fluid principal properties of example 1, comparative examples 1-2
The sand suspension performance detection is carried out according to the following steps: 500mL of the fracturing fluid of the embodiment 1, the fracturing fluid of the comparative embodiment 1-2, the conventional slickwater fracturing fluid A and the conventional slickwater fracturing fluid B are respectively poured into a Wu-Ying mixer, 150g of 40-70 mesh ceramsite is added into a Wu Yinhun mixer, and the mixture is stirred at a stirring speed of 500 revolutions per minute for 2 minutes and then is immediately poured into a 1000mL measuring cylinder, timing is started, the sedimentation condition of the ceramsite is recorded, and the sand suspending performance of the fracturing fluid is characterized. The slower the ceramsite subsides, the better the sand suspending performance of the fracturing fluid. The results of sand suspension performance test are shown in Table 2.
Table 2 fracturing fluid sand suspending properties of example 1, comparative examples 1-2
As can be seen from the above tables 1 and 2, compared with the example 1, the comparative example 1-1 has a significantly reduced removal rate (62% to 42%) after removing the nanoemulsion in the fracturing fluid formulation, which indicates that the nanoemulsion in the example 1 can improve the flowing property of the fracturing fluid in the micro-cracks and the flowback rate by dialysis and the like, which is very beneficial to reducing the damage of the fracturing fluid; other properties were not significantly changed.
Comparative examples 1-2 compared with example 1, after the nanoemulsion composition is changed in the fracturing fluid formulation (the gemini fluorocarbon surfactant is removed, and the ultrasonic treatment is removed), the rejection rate is greatly reduced (62% is reduced to 45%), which shows that the nanoemulsion in example 1 can improve the flow property of the fracturing fluid in micro-cracks and the flowback rate through dialysis and the like, and is very beneficial to reducing the damage of the fracturing fluid; other properties were not significantly changed; the nanoemulsions of comparative examples 1-2 did not achieve the same effect as the nanoemulsion of example 1.
Compared with the conventional slickwater fracturing fluid A, B, the resistivity is reduced by 2.1 percent and 10.1 percent respectively, and the sand suspending performance is half of that of the fracturing fluid of the embodiment 1 from '20 s later, 3min, and 10min after the complete settlement' is changed into '0 s later, and 10s after the complete settlement', which shows that the fracturing fluid of the embodiment 1 improves the resistivity of the low-viscosity slickwater fracturing fluid and greatly improves the sand suspending performance of the low-viscosity slickwater fracturing fluid.
Example 2
The embodiment provides an integrated fracturing fluid, which comprises the following components in percentage by mass: 0.2% of a resistance-reducing tackifier, 0.2% of a nano emulsion, 0.03% of a nonionic fluorocarbon surfactant, 0.004% of a bactericide, 0.2% of a clay stabilizer, 0.02% of a gel breaker, 0.1% of a modifier, 0.3% of a gas generator and the balance of water.
The viscosity-reducing tackifier is a mixture of polyacrylamide with viscosity-average molecular weight of 1170 ten thousand and hydrolysis degree of 28% and non-hydrolyzed polyacrylamide with viscosity-average molecular weight of 1150 ten thousand, and the mass ratio of the two is 14:1.
The nanoemulsion is a nanoemulsion with an average particle size of 130 nm. Based on 100% of the total mass of the nanoemulsion, the nanoemulsion comprises: 18% hydroxy fluorosilicone oil (Wohan British Biotechnology Co., ltd.) and 7% Gemini fluorocarbon surfactant C 2 F 5 N + (CH 3 ) 2 -CH 2 CH 2 CH 2 CH 2 -(CH 3 ) 2 N + C 2 F 5 (self-made: 1.5 parts of pentafluorobromide is added into 7 parts of acetone at 30 ℃ in parts by weight, uniformly mixed under stirring at 150rpm, 1 part of tetramethylbutanediamine is added dropwise, completely and uniformly added for 12min, quaternization reaction is carried out under stirring at 150rpm, after reaction for 1.5 hours, the obtained precipitate is filtered and precipitated, and the obtained precipitate is the prepared binary fluorocarbon surfactant), 20% of nonionic fluorocarbon surfactant (FCF-204, guangzhou Shunchun new material science and technology Co., ltd.), 5% of nano silicon dioxide with average particle size of 20nm, 7% of ethanol and the balance of water.
The nanoemulsion is prepared by the following steps: the above-mentioned nanometerThe content of each component in the rice emulsion is added with water in a reaction kettle, and the gemini fluorocarbon surfactant C is stirred at 35 ℃ and 300rpm 2 F 5 N + (CH 3 ) 2 -CH 2 CH 2 CH 2 CH 2 -(CH 3 ) 2 N + C 2 F 5 Adding the nonionic fluorocarbon surfactant into the reaction kettle, and stirring for 30min; adding ethanol, and stirring for 15min; adding nano silicon dioxide, and continuing stirring for 20min; dripping hydroxyfluorosilicone oil at a speed of 30min after uniform dripping, and continuously stirring for 45min; finally, ultrasonic treatment with the frequency of 16 kilohertz is adopted for 30 minutes to obtain the nano emulsion.
The nonionic fluorocarbon surfactant is FCF-204 of Guangzhou Shunchun New Material technology Co.
The bactericide is dodecyl trimethyl ammonium chloride.
The clay stabilizer is polyquaternium.
The gel breaker is potassium persulfate.
The modifier is 3-aminopropyl triethoxy silane.
The specific preparation steps of the effervescent tablet granule with the acid source of citric acid, the alkali source of sodium bicarbonate and the polyethylene glycol as the coating are the same as those of the example 1.
The preparation method of the integrated fracturing fluid of the embodiment comprises the following steps: slowly adding 0.2% of the resistance-reducing tackifier into water under the stirring condition of 150 revolutions per minute, and uniformly stirring and mixing; then sequentially adding 0.004% of the bactericide, 0.2% of the clay stabilizer, 0.1% of the modifier, 0.2% of the nano emulsion and 0.03% of the nonionic fluorocarbon surfactant, and stirring and mixing uniformly; and finally, adding 0.3% of the gas generating agent and 0.02% of the gel breaker, and uniformly stirring to obtain the integrated fracturing fluid.
Comparative example 2
The fracturing fluid of comparative example 2 was obtained by removing the modifier and the gas generating agent from the fracturing fluid components of example 2, and the remaining components and contents and the fracturing fluid preparation method were the same.
Conventional linear fracturing fluid C:
based on 100% of the total mass of the conventional linear adhesive fracturing fluid C, the linear adhesive fracturing fluid C is prepared from 0.4% of polyacrylamide emulsion with 990 ten thousand viscosity average molecular weight and a degree of hydrolysis of 25% (Chengdu Tech development Co., ltd., CT 1-20D), 0.1% of a drainage aid (Chengdu Tech development Co., ltd., CT 5-12), 0.005% of a bactericide (Chengdu Tech development Co., ltd., CT 10-4) and the balance of water.
Conventional linear fracturing fluid D:
based on the total mass of the conventional linear adhesive fracturing fluid D being 100%, the conventional linear adhesive fracturing fluid D is prepared from 0.25% of hydrophobic association polymer powder with viscosity average molecular weight of 880 ten thousand (Chengsheng Tech development Co., ltd., CT 1-20B), 0.1% of drainage aid (Chengsheng Tech development Co., ltd., CT 5-12), 0.005% of bactericide (Chengsheng Tech development Co., ltd., CT 10-4) and the balance of water.
The fracturing fluids prepared in example 2 and comparative example 2 are medium viscosity fracturing fluids, and the main properties of the fracturing fluids are as described in line standard NB/T14003.3-2017, shale gas fracturing fluid part 3: the performance index and evaluation method of the continuous mixed fracturing fluid detect that the bacterial content is according to line standard NB/T14003.1-2015, shale gas fracturing fluid part 1: the performance index of slick water and the evaluation method. The results of the main properties of the fracturing fluid are shown in Table 3. Sand suspension performance test was performed according to the test method of example 1, and the test results are shown in table 4.
TABLE 3 fracturing fluid principal properties of example 2 and comparative example 2
Table 4 fracturing fluid sand suspending properties of example 2 and comparative example 2
As can be seen from the above tables 3 and 4, compared with the example 2, the comparative example 2 has the discharge rate reduced from 55% to 45% after the modifier and the gas generating agent are removed from the fracturing fluid formulation, which indicates that the modifier and the gas generating agent in the example 2 can improve the flowing property of the fracturing fluid in the micro-cracks and increase the flowback rate by generating gas energization; meanwhile, after the modifier and the gas generating agent are removed from the fracturing fluid formula of the comparative example 2, the sand suspending performance is changed from '1 min later to 5min later to half after the fracturing fluid is settled, no obvious continuous settlement phenomenon is generated from 5min to 10 min' to '2 s later to begin settlement, 30s to half after settlement and 90s to complete settlement', which indicates that the fracturing fluid of the example 2 greatly improves the sand suspending performance of the medium viscosity slick water fracturing fluid; other properties were not significantly changed.
Compared with the embodiment 2, the conventional linear adhesive fracturing fluid C, D has the advantages that the resistivity is reduced by 7.3 percent and 2.3 percent respectively, the sand suspension performance is half of that of the embodiment 2 from the initial sedimentation after 1min, the initial sedimentation after 5min, the sedimentation after 5min to 10min without obvious continuous sedimentation phenomenon is changed into 2s, the sedimentation after 20s is half, and the complete sedimentation after 1min, so that the fracturing fluid of the embodiment 2 improves the resistivity of the medium-viscosity slick water, and the sand suspension performance of the low-viscosity slick water fracturing fluid is greatly improved.
Example 3
The embodiment provides an integrated fracturing fluid, which comprises the following components in percentage by mass: 0.3% of a resistance-reducing tackifier, 0.3% of a nano emulsion, 0.05% of a nonionic fluorocarbon surfactant, 0.01% of a bactericide, 0.3% of a viscosity regulator, 0.2% of a clay stabilizer, 0.08% of a gel breaker, 0.15% of a modifier, 0.2% of a gas generator and the balance of water.
The viscosity-reducing tackifier is a mixture of polyacrylamide with viscosity-average molecular weight of 810 ten thousand and hydrolysis degree of 22% and non-hydrolyzed polyacrylamide with viscosity-average molecular weight of 780, and the mass ratio of the two is 10:1.
The nanoemulsion is a nanoemulsion with an average particle size of 130 nm. Based on 100% of the total mass of the nanoemulsion, the nanoemulsion comprises: 15% vinyl fluorosilicone oil (KX-205, guangzhou Kangxi organosilicon materials Co., ltd.) and 5% Gemini fluorocarbon surfactant C 2 F 5 N + (CH 3 ) 2 -CH 2 CH 2 CH 2 CH 2 -(CH 3 ) 2 N + C 2 F 5 (self-made: 1.5 parts of pentafluorobromide is added into 7 parts of acetone at 30 ℃ in parts by weight, uniformly mixed under stirring at 150rpm, 1 part of tetramethylbutanediamine is added dropwise, completely and uniformly added for 12min, quaternization reaction is carried out under stirring at 150rpm, after reaction for 1.5 hours, the obtained precipitate is filtered, and the obtained precipitate is the prepared binary fluorocarbon surfactant), 20% of nonionic fluorocarbon surfactant (3M company, FC 4430), 5% of nano silicon dioxide with the average particle size of 30nm, 9% of propanol and the balance of water.
The nanoemulsion is prepared by the following steps: according to the content of each component in the nano emulsion, adding water into a reaction kettle, stirring at 30 ℃ and 300rpm to obtain the gemini fluorocarbon surfactant C 2 F 5 N + (CH 3 ) 2 -CH 2 CH 2 CH 2 CH 2 -(CH 3 ) 2 N + C 2 F 5 Adding the nonionic fluorocarbon surfactant into the reaction kettle, and stirring for 15min; adding propanol, and stirring for 20min; adding nano silicon dioxide, and continuing stirring for 25min; dripping vinyl fluorosilicone oil at a speed of 30min after uniform dripping, and continuously stirring for 40min; finally, ultrasonic treatment with the frequency of 18 kilohertz is adopted for 25 minutes to obtain the nano emulsion.
The nonionic fluorocarbon surfactant is FC4430 from 3M company.
The bactericide is methyl isothiazolinone.
The viscosity modifier is a complex obtained by complexing zirconium oxychloride with sorbitol. The preparation method comprises the following steps: mixing zirconium oxychloride and sorbitol with water according to the weight ratio of zirconium oxychloride to sorbitol being 20:50:30, and carrying out complexation reaction for 1h at 60 ℃ to obtain the viscosity regulator.
The clay stabilizer is potassium chloride.
The breaker is ammonium persulfate.
The modifier is N-beta-aminoethyl-gamma-aminopropyl trimethoxy silane.
The specific preparation steps of the effervescent tablet granule with the acid source of citric acid, the alkali source of sodium bicarbonate and the polyethylene glycol as the coating are the same as those of the example 1.
The preparation method of the integrated fracturing fluid of the embodiment comprises the following steps: slowly adding 0.3% of the resistance-reducing tackifier into water under the stirring condition of 150 revolutions per minute, and uniformly stirring and mixing; then sequentially adding 0.01% of the bactericide, 0.2% of the clay stabilizer, 0.15% of the modifier, 0.3% of the nanoemulsion and 0.05% of the nonionic fluorocarbon surfactant, and stirring and mixing uniformly; adding 0.3% of the viscosity modifier, and stirring and mixing uniformly; and finally, adding 0.2% of the gas generating agent and 0.08% of the gel breaker, and uniformly stirring to obtain the integrated fracturing fluid.
Comparative example 3-1
In the fracturing fluid components of example 3, 0.3% of the resistance-reducing tackifier is completely replaced by hydrolyzed polyacrylamide (non-hydrolyzed polyacrylamide) with the molecular weight of 810 ten thousand and the hydrolysis degree of 22%, and the rest components, the content and the preparation method of the fracturing fluid are the same, so that the fracturing fluid of comparative example 3-1 is obtained.
Comparative example 3-2
In the fracturing fluid components of the embodiment 3, the mass percentage of the resistance-reducing tackifier in the fracturing fluid is replaced by 0.7%, and the rest components and contents are the same as those of the fracturing fluid preparation method, so that the fracturing fluid of the comparative example 3-2 is obtained.
Conventional gel fracturing fluid E:
based on 100% of the total mass of the conventional gel fracturing fluid E, the gel fracturing fluid E is prepared from 0.4% of polyacrylamide emulsion with 990 ten thousand viscosity average molecular weight and a degree of hydrolysis of 25% (Chengshi Tech development Co., ltd., CT 1-20D), 0.1% of a drainage aid (Chengshi Tech development Co., ltd., CT 5-12), 0.005% of a bactericide (Chengshi Tech development Co., ltd., CT 10-4), 0.4% of an organozirconium crosslinking agent (which is the same as the viscosity regulator of example 3) and the balance of water.
Conventional gel fracturing fluid F:
based on the total mass of the conventional gel fracturing fluid F being 100%, the gel fracturing fluid F is prepared from 0.25% of hydrophobic association polymer powder with viscosity average molecular weight of 880 ten thousand (Chengshi Tech development Co., ltd., CT 1-20B), 0.1% of a drainage aid (Chengshi Tech development Co., ltd., CT 5-12), 0.005% of a bactericide (Chengshi Tech development Co., ltd., CT 10-4), 0.4% of an organozirconium cross-linking agent (which is the same as the viscosity regulator of example 3) and the balance of water.
The fracturing fluids prepared in the embodiment 3 and the comparative examples 3-1 and 3-2 are high-viscosity fracturing fluids, and the main performances of the fracturing fluids are as follows from line standard NB/T14003.3-2017, shale gas fracturing fluid part 3: the performance index and evaluation method of the continuous mixed fracturing fluid detect that the bacterial content is according to line standard NB/T14003.1-2015, shale gas fracturing fluid part 1: the performance index of slick water and the evaluation method. The results of the main properties of the fracturing fluid are shown in Table 5. Sand suspension performance test was performed according to the test method of example 1, and the test results are shown in table 6.
TABLE 5 fracturing fluid principal properties of example 3, comparative example 3-1, comparative example 3-2
TABLE 6 fracturing fluid sand suspending Properties of example 3 and comparative examples 3-1 and 3-2
As can be seen from the above tables 5 and 6, compared with the example 3, the comparative example 3-1 shows that after the viscosity-reducing agent in the fracturing fluid formulation is completely replaced by the hydrolyzed polyacrylamide (without non-hydrolyzed polyacrylamide), the resistivity is reduced from 71.2% to 61.1%, which indicates that the non-hydrolyzed polyacrylamide in the example 3 does not participate in the crosslinking, and can maintain the linear polymer state, thereby ensuring the high resistivity, and the hydrolyzed polyacrylamide participates in the crosslinking, becomes a space network structure, so that the resistivity is reduced; other properties were not significantly changed.
Compared with the embodiment 3, the comparative example 3-2 has the advantages that after the concentration of the resistance-reducing tackifier in the fracturing fluid formulation is increased to 0.7%, the resistance-reducing rate is reduced from 71.2% to 35.1%, and the fracturing fluid is stirred after the gel is formed, the whole gel cannot be recovered, and the fact that the excessive concentration of the resistance-reducing tackifier can cause cross-linking, the gel is fragile, the friction resistance of the fracturing fluid is increased, and the resistance-reducing rate is reduced is shown.
Compared with the conventional gel fracturing fluid E, F in the embodiment 3, the resistivity is reduced by 11.2 percent and 6.2 percent respectively, and the sand suspending performance is changed from 'no obvious sedimentation phenomenon in 10 min' in the embodiment 3 to '10 min sedimentation 10% of ceramsite', which indicates that the embodiment 3 greatly improves the resistivity reducing performance and the sand suspending performance of the high-viscosity gel fracturing fluid.
Example 4
The embodiment provides an integrated fracturing fluid, which comprises the following components in percentage by mass: 0.4% of a resistance-reducing tackifier, 0.4% of a nano emulsion, 0.08% of a nonionic fluorocarbon surfactant, 0.03% of a bactericide, 0.3% of a viscosity regulator, 0.4% of a clay stabilizer, 0.1% of a gel breaker, 0.15% of a modifier, 0.3% of a gas generator and the balance of water.
The viscosity-reducing tackifier is a mixture of polyacrylamide with a viscosity-average molecular weight of 1210 ten thousand and a hydrolysis degree of 30% and non-hydrolyzed polyacrylamide with a viscosity-average molecular weight of 1140, and the mass ratio of the two is 13:1.
The nanoemulsion is a nanoemulsion with an average particle size of 150 nm. Based on 100% of the total mass of the nanoemulsion, the nanoemulsion comprises: 8% hydroxy fluorosilicone oil (Wuhan Rong and lautness biotechnology Co., ltd.), 7% vinyl fluorosilicone oil (KX-205, guangzhou Kangxi organosilicon materials Co., ltd.), 8% gemini fluorocarbon surfactant C 2 F 5 N + (CH 3 ) 2 -CH 2 CH 2 CH 2 CH 2 -(CH 3 ) 2 N + C 2 F 5 (self-made: 1.5 parts of pentafluorobromide ethane was added to 7 parts of acetone in parts by weight at 30 ℃ C., and mixed uniformly with stirring at 150rpm, and then droppedAdding 1 part of tetramethylbutanediamine, uniformly dropwise adding for 12min, performing quaternization reaction under stirring at 150rpm, filtering the precipitate after reacting for 1.5h, and obtaining the precipitate which is the prepared gemini fluorocarbon surfactant), 18% of nonionic fluorocarbon surfactant (3M company, FC 4432), 8% of nano silicon dioxide with the average particle size of 40nm, 6% of ethanol and the balance of water.
The nanoemulsion is prepared by the following steps: according to the content of each component in the nano emulsion, adding water into a reaction kettle, and stirring at 35 ℃ and 500rpm to obtain the gemini fluorocarbon surfactant C 2 F 5 N + (CH 3 ) 2 -CH 2 CH 2 CH 2 CH 2 -(CH 3 ) 2 N + C 2 F 5 Adding the nonionic fluorocarbon surfactant into the reaction kettle, and stirring for 15min; adding propanol, and stirring for 20min; adding nano silicon dioxide, and continuing stirring for 20min; respectively dripping hydroxyl fluorosilicone oil and vinyl fluorosilicone oil at a speed of 30min after uniform dripping, and continuously stirring for 35min; finally, ultrasonic treatment with the frequency of 30 kilohertz is adopted for 35 minutes to obtain the nano emulsion.
The nonionic fluorocarbon surfactant is FC4432 from 3M company.
The bactericide is dodecyl dimethyl benzyl ammonium bromide.
The viscosity modifier is a complex obtained by complexation reaction of diisopropyl di (triethanolamine) titanate and glycerol. The preparation method comprises the following steps: and mixing the diisopropyl di (triethanolamine) titanate, the glycerol and the water according to the weight ratio of the diisopropyl di (triethanolamine) titanate to the glycerol to the water of 25:38:37, and carrying out complexation reaction for 2 hours at 70 ℃ to obtain the viscosity regulator.
The clay stabilizer is tetramethyl ammonium chloride.
The gel breaker is sodium persulfate.
The modifier is 3-aminopropyl triethoxy silane.
The specific preparation steps of the effervescent tablet granule with the acid source of citric acid, the alkali source of sodium bicarbonate and the polyethylene glycol as the coating are the same as those of the example 1.
The preparation method of the integrated fracturing fluid of the embodiment comprises the following steps: slowly adding 0.4% of the resistance-reducing tackifier into water under the stirring condition of 180 revolutions per minute, and uniformly stirring and mixing; then sequentially adding 0.03% of the bactericide, 0.4% of the clay stabilizer, 0.15% of the modifier, 0.4% of the nanoemulsion and 0.08% of the nonionic fluorocarbon surfactant, and stirring and mixing uniformly; adding 0.3% of the viscosity modifier, and stirring and mixing uniformly; and finally, adding 0.3% of the gas generating agent and 0.1% of the gel breaker, and uniformly stirring to obtain the integrated fracturing fluid.
The fracturing fluids prepared in the example 4 and the example 3, the comparative example 3-1 and the comparative example 3-2 are high-viscosity fracturing fluids, and the main performances of the fracturing fluids are as follows from line standard NB/T14003.3-2017, shale gas fracturing fluid part 3: the performance index and evaluation method of the continuous mixed fracturing fluid detect that the bacterial content is according to line standard NB/T14003.1-2015, shale gas fracturing fluid part 1: the performance index of slick water and the evaluation method. The results of the main properties of the fracturing fluid are shown in Table 7. Sand suspension performance test was performed according to the test method of example 1, and the test results are shown in table 8.
Table 7 major properties of fracturing fluids of example 4, example 3, comparative example 3-1, comparative example 3-2
Table 8 fracturing fluid sand suspending properties of example 4, example 3, comparative example 3-1, comparative example 3-2
As can be seen from the above tables 7 and 8, the fracturing fluid of example 4 was comparable in performance to example 3.
In summary, under the same viscosity, the fracturing fluid provided by the invention has higher sand suspending performance than the conventional fracturing fluid, in particular to a low-viscosity slickwater fracturing fluid and a medium-viscosity linear gel fracturing fluid. Compared with the conventional fracturing fluid, the fracturing fluid provided by the invention has the advantages that the friction resistance is lower, the resistivity is improved by 2.1-11.2 percent, and the higher the viscosity is, the larger the amplitude of the resistivity improvement is. Meanwhile, the sand suspension performance of the fracturing fluid provided by the invention is superior to that of conventional fracturing fluid with the same viscosity, and particularly in the provided high-viscosity gel fracturing fluid, the sand suspension does not settle within 10min (in the conventional gel fracturing fluid with the same viscosity, the sand suspension settles for 10% within 10 min).

Claims (17)

1. The integrated fracturing fluid comprises the following components in percentage by mass: 0.02-0.5% of resistance-reducing tackifier, 0.1-0.5% of nano emulsion, 0.02-0.1% of first nonionic fluorocarbon surfactant, 0.003-0.05% of bactericide, 0-0.5% of viscosity regulator, 0-0.5% of clay stabilizer, 0-0.1% of gel breaker, 0.05-0.2% of modifier, 0.1-1% of gas producer and the balance of water;
preferably, when the integrated fracturing fluid contains a viscosity modifier, the content of the viscosity modifier is 0.1-0.5% based on 100% of the total mass of the integrated fracturing fluid;
preferably, when the integrated fracturing fluid contains a breaker, the content of the breaker is 0.02-0.1% based on 100% of the total mass of the integrated fracturing fluid;
preferably, when the integrated fracturing fluid contains a clay stabilizer, the content of the clay stabilizer is 0.01-0.5% based on 100% of the total mass of the integrated fracturing fluid.
2. The integrated fracturing fluid of claim 1, wherein the drag reducing tackifier is a mixture of hydrolyzed polyacrylamide and/or derivatives thereof and non-hydrolyzed polyacrylamide and/or derivatives thereof; preferably, the mass ratio of the hydrolyzed polyacrylamide and/or derivative thereof to the non-hydrolyzed polyacrylamide and/or derivative thereof is (10-15): 1.
3. The integrated fracturing fluid of claim 2, wherein in the drag reducing tackifier, the hydrolyzed polyacrylamide and/or derivative thereof has a viscosity average molecular weight of 500-1500 tens of thousands and a degree of hydrolysis of 20% -30%; the viscosity average molecular weight of the non-hydrolytic polyacrylamide and/or the derivative thereof is 500 ten thousand to 1500 ten thousand.
4. The integrated fracturing fluid of claim 1, wherein the nanoemulsion is a nanoemulsion having an average particle diameter of less than or equal to 150 nm;
preferably, it comprises the following components, based on 100% of the total mass of the nanoemulsion: 10% -20% of fluorine-containing silicone oil, 5% -10% of gemini fluorocarbon surfactant, 15% -25% of second nonionic fluorocarbon surfactant, 5% -10% of nano silicon dioxide, 1% -10% of lower alcohol and the balance of water;
more preferably, the fluorine-containing silicone oil comprises one or a combination of a plurality of hydroxyl fluorine silicone oil, vinyl fluorine silicone oil, methyl fluorine silicone oil and polyether fluorine silicone oil;
more preferably, the gemini fluorocarbon surfactant has the structural formula: c (C) n F 2n+1 N + (CH 3 ) 2 -CH 2 CH 2 CH 2 CH 2 -(CH 3 ) 2 N + C n F 2n+1 Wherein n is 2-4;
more preferably, the second nonionic fluorocarbon surfactant comprises one or a combination of several of polyoxyethylene ether of fluorine-containing fatty alcohol, polyoxyethylene ether of fluorine-containing phenol, polyoxyethylene ether of fluorine-containing alkyl sulfonyl alcohol amine, polyoxyethylene ester of fluorine-containing carboxylic acid and polyoxyethylene ether of fluorine-containing thiol;
More preferably, the nano-silica has a particle size of 15-50nm;
more preferably, the lower alcohol comprises one or a combination of several of methanol, ethanol, propanol and butanol.
5. The integrated fracturing fluid of claim 4, wherein the nanoemulsion is prepared by the steps of: adding a gemini fluorocarbon surfactant and a nonionic fluorocarbon surfactant into water according to the content of each component in the nano emulsion at the stirring speed of 120-600rpm at the temperature of 10-40 ℃, and then stirring for 10-30min; adding lower alcohol, and stirring for 10-30min; adding nano silicon dioxide, and continuing stirring for 10-30min; dripping fluorine-containing silicone oil, and continuously stirring for 30-60min; finally, ultrasonic treatment is carried out for 20-40min, and the nano emulsion is obtained.
6. The integrated fracturing fluid of claim 1, wherein the first nonionic fluorocarbon surfactant comprises one or a combination of several of a polyoxyethylene ether of a fluorine-containing fatty alcohol, a polyoxyethylene ether of a fluorine-containing phenol, a polyoxyethylene ether of a fluorine-containing alkyl sulfonyl alcohol amine, a polyoxyethylene ester of a fluorine-containing carboxylic acid, and a polyoxyethylene ether of a fluorine-containing thiol.
7. The integrated fracturing fluid of claim 1, wherein the bactericide comprises one or a combination of several of aldehyde bactericides, quaternary ammonium salt bactericides and isothiazolinone bactericides;
Preferably, the aldehyde germicide comprises one or a combination of more of glutaraldehyde, formaldehyde and acrolein;
preferably, the quaternary ammonium salt bactericide comprises one or a combination of more of tetradecyldimethylbenzyl ammonium chloride, dodecyl trimethyl ammonium chloride, dodecyl dimethylbenzyl ammonium chloride and dodecyl dimethylbenzyl ammonium bromide;
preferably, the isothiazolinone bactericides include methyl isothiazolinone and/or methyl chloroisothiazolinone.
8. The integrated fracturing fluid of claim 1, wherein the viscosity modifier comprises one or a combination of several of a water-soluble zirconium salt, a water-soluble titanium salt, a water-soluble chromium salt, and a water-soluble aluminum salt;
preferably, the viscosity modifier comprises: and the water-soluble zirconium salt, the water-soluble titanium salt, the water-soluble chromium salt and the water-soluble aluminum salt are respectively subjected to complexation reaction with polyhydroxy alcohol to obtain one or a combination of a plurality of water-soluble organic zirconium salts, water-soluble organic titanium salts, water-soluble organic chromium salts and water-soluble organic aluminum salts.
9. The integrated fracturing fluid of claim 8, wherein the water-soluble organozirconium salt comprises a complex of zirconium oxychloride with one or more of sorbitol, glycerol, ethylene glycol, 1, 2-propanediol, 1, 4-butanediol, diethylene glycol, and triethylene glycol.
10. The integrated fracturing fluid of claim 8, wherein the water-soluble organic titanium salt comprises one or a combination of several of diisopropyl di (triethanolamine) titanate, tetraisopropyl orthotitanate, diisopropyl orthotitanate, and diisopropyl orthotitanate; or a complex obtained by complexation reaction of one or more of diisopropyl di (triethanolamine) titanate, tetraisopropyl orthotitanate, diisopropyl orthotitanate and diisopropyl orthotitanate with one or more of sorbitol, glycerol, ethylene glycol, 1, 2-propylene glycol, 1, 4-butanediol, diethylene glycol and triethylene glycol.
11. The integrated fracturing fluid of claim 8, wherein the water-soluble organic chromium salt comprises a complex obtained by complexation of one or more of chromium lactate, chromium acetate, chromium chloride, and chromium sulfate with one or more of sorbitol, glycerol, ethylene glycol, 1, 2-propanediol, 1, 4-butanediol, diethylene glycol, and triethylene glycol.
12. The integrated fracturing fluid of claim 8, wherein the water-soluble organic aluminum salt comprises a complex obtained by complexation of one or more of aluminum potassium sulfate dodecahydrate, aluminum sulfate, aluminum lactate, aluminum acetate, and aluminum chloride with one or more of sorbitol, glycerol, ethylene glycol, 1, 2-propanediol, 1, 4-butanediol, diethylene glycol, and triethylene glycol.
13. The integrated fracturing fluid of claim 1, wherein the clay stabilizer comprises one or a combination of several of tetramethyl ammonium chloride, potassium chloride, and polyquaternium.
14. The integrated fracturing fluid of claim 1, wherein the breaker comprises one or a combination of several of ammonium persulfate, sodium persulfate, and potassium persulfate.
15. The integrated fracturing fluid of claim 1, wherein the modifier comprises a silane modifier; preferably, the silane modifier comprises one or a combination of several of N-beta-aminoethyl-gamma-aminopropyl methyl dimethoxy silane, 3-aminopropyl triethoxy silane and N-beta-aminoethyl-gamma-aminopropyl trimethoxy silane.
16. The integrated fracturing fluid of claim 1, wherein the gas generating agent comprises effervescent tablet particles; preferably, the effervescent tablet particles are effervescent tablet particles with acid source of citric acid, alkali source of sodium bicarbonate and polyethylene glycol as coating.
17. A method of preparing the integrated fracturing fluid of any of claims 1-16, comprising the steps of:
when indoor preparation is carried out:
s1, adding 0.02% -0.5% of resistance-reducing tackifier into water under the stirring condition of 60-200 rpm, and stirring and mixing uniformly, wherein the total mass of the integrated fracturing fluid is 100%;
S2, adding 0.003% -0.05% of bactericide, 0-0.5% of clay stabilizer, 0.05% -0.2% of modifier, 0.1% -0.5% of nano emulsion and 0.02% -0.1% of first nonionic fluorocarbon surfactant, and uniformly stirring and mixing to obtain a first mixed solution;
s3, adding 0-0.5% of viscosity regulator into the first mixed solution according to the viscosity requirement of the required fracturing fluid, and uniformly stirring and mixing to obtain a second mixed solution;
s4, adding 0.1-1% of gas generating agent and 0-0.1% of gel breaker into the second mixed solution, and uniformly stirring to obtain the integrated fracturing fluid;
when formulated in situ:
the preparation steps of S1-S3 are the same as those of indoor preparation, and the preparation steps of S4 are as follows: adding 0.1% -1% of gas generating agent and 0-0.1% of gel breaker into a sand mixing tank of a sand mixing vehicle, and uniformly mixing the gas generating agent, the gel breaker, the second mixed solution and sand in the sand mixing tank of the sand mixing vehicle.
CN202210793627.1A 2022-07-07 2022-07-07 Integrated fracturing fluid and preparation method thereof Pending CN117402602A (en)

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