CN112480900A - Viscoelastic long-carbon-chain amine oxide micelle fracturing fluid resistant to temperature of 150 DEG C - Google Patents
Viscoelastic long-carbon-chain amine oxide micelle fracturing fluid resistant to temperature of 150 DEG C Download PDFInfo
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- CN112480900A CN112480900A CN202011483599.0A CN202011483599A CN112480900A CN 112480900 A CN112480900 A CN 112480900A CN 202011483599 A CN202011483599 A CN 202011483599A CN 112480900 A CN112480900 A CN 112480900A
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- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/60—Compositions for stimulating production by acting on the underground formation
- C09K8/62—Compositions for forming crevices or fractures
- C09K8/66—Compositions based on water or polar solvents
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- C09K8/60—Compositions for stimulating production by acting on the underground formation
- C09K8/602—Compositions for stimulating production by acting on the underground formation containing surfactants
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- C—CHEMISTRY; METALLURGY
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- C09K2208/30—Viscoelastic surfactants [VES]
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Abstract
The invention relates to a long-carbon-chain amine oxide type clean fracturing fluid and a preparation method thereof, and belongs to the key technical field of oil field chemical development and oil gas fracturing development. Oxidizing oleamide propyl dimethyl tertiary amine and erucic acid amide propyl dimethyl tertiary amine by hydrogen peroxide to prepare long-carbon-chain amine oxide, and compounding the long-carbon-chain amine oxide with a counter ion salt to obtain the viscoelastic micelle fracturing fluid. The complex viscoelastic long carbon chain amine oxide micelle fracturing fluid prepared by the method is sheared for 60min at the temperature of 150 ℃, and the retained viscosity is 59.50mPa & s. The amine oxide type clean fracturing fluid provided by the invention is simple in preparation process and good in rheological property, and is expected to be rich in high-temperature-resistant viscoelastic surfactant fracturing fluid.
Description
Technical Field
The invention relates to the key technical field of oilfield chemical development and oil-gas fracturing development, in particular to viscoelastic long-carbon-chain amine oxide micelle fracturing fluid capable of resisting temperature of 150 ℃.
Background
China is an important world petroleum import country, and over 70 percent of crude oil in China depends on import. As conventional oil and gas reservoirs are continuously developed and consumed, unconventional high-temperature low-permeability reservoirs are urgently developed and utilized. Fracturing remains the most commonly selected construction process for developing such unconventional reservoirs. The hydraulic fracturing technology is a reservoir transformation technology which is characterized in that a fracturing fluid is injected into the ground from a shaft through high-pressure equipment on the ground, the fracturing fluid carries a propping agent, and one or more fractures with flow conductivity are formed below the ground, so that the yield increase and the stable yield of an oil-gas field are realized.
The current common high-temperature-resistant fracturing liquid system comprises polymer fracturing liquid and has the problems of incomplete gel breaking, low flowback rate, great damage to stratum and the like. The clean fracturing fluid system taking the surfactant as the thickening agent is simple to prepare, does not need to be crosslinked, can automatically break gel, has no residue in gel breaking liquid, and has small damage to the stratum. However, the clean fracturing fluid proposed in the early stage has poor temperature resistance, and the application of the clean fracturing fluid in high-temperature deep reservoirs is greatly limited. At present, the clean fracturing fluid applicable to medium and high temperature reservoirs has fewer formulas and is expensive.
The high temperature viscoelastic micelle systems reported so far mainly include cationic surfactants based on quaternary ammonium salt surfactants [ Jiang B, Zhang D, Li D P, et al. Performance of temperature resistant VES reactive fluidized SCF. oil field Chemistry,2003,20(4): 332) 334], anionic surfactants based on sulfate and sulfonate types [ Yang G K, Yang J, Guan B S, et al. high temperature reactive fluidized and low temperature resistant VES HT01 reactive fluidized bed Chemistry, oil field Chemistry,2014,31(1):29-32], amphoteric surfactants based on betaine type [ Wang H M, Dai C L, Yi Q, pressure of temperature resistant micelles, and novel surfactants [ 70, 84 ] having the structures of quaternary ammonium salt surfactants [ fresh G K, oil J, oil K, oil surfactant, oil, surfactant, yang X J, Song Z F, et al, development and performance evaluation of high temperature and clean fragmented fluid system HT-160, Petroleum Drilling techniques.2017,45(6):105-109], but no studies of high temperature 150 ℃ resistant viscoelastic amine oxide micellar fracturing fluids have been reported.
The amine oxide type surfactant has the characteristics of simple and direct synthesis process, almost no toxicity and the like, and when the length of a hydrophobic carbon chain in the structural formula of the surfactant is more than or equal to 18, the viscoelastic surfactant fracturing fluid with good performance is expected to be obtained.
Disclosure of Invention
The invention aims to provide a preparation method of viscoelastic long-carbon-chain amine oxide micelle fracturing fluid capable of resisting temperature of 150 ℃, which is applicable to oil and gas field reservoirs at about 150 ℃.
The invention is realized by the following technical scheme:
the viscoelastic long-carbon-chain amine oxide micelle fracturing fluid capable of resisting the temperature of 150 ℃ is characterized by being prepared by the following method, and comprises the following steps:
1) preparing a long-carbon-chain amine oxide thickening agent:
a. mixing 6 wt% disodium ethylene diamine tetraacetate (6 wt% EDTA-2 Na) water solution with anhydrous methanol and water, stirring,
b. b, adding oleamide propyl dimethyl tertiary amine and erucic acid amide propyl dimethyl tertiary amine into the solution prepared in the step a, uniformly stirring, and preparing a mixed tertiary amine solution;
wherein, EDTA-2 Na aqueous solution: anhydrous methanol: water: mass ratio of mixed tertiary amine 1.2%: 40.4%: 1.2%: 57.2 percent, the total mole number of the oleic acid amide propyl dimethyl tertiary amine and the erucic acid amide propyl dimethyl tertiary amine is 0.1 mole, and the mole ratio of the oleic acid amide propyl dimethyl tertiary amine to the erucic acid amide propyl dimethyl tertiary amine is 0: 1-1: 0;
c. adding 30 wt% of hydrogen peroxide into the mixed tertiary amine solution in the step b, wherein the molar ratio of the hydrogen peroxide to the mixed tertiary amine is 1.15:1.0, and oxidizing for 5-7 hours by the hydrogen peroxide at the temperature of 50-70 ℃ to prepare a long-carbon-chain amine oxide thickening agent;
2) mixing and compounding the long-carbon-chain amine oxide thickening agent, the counter-ion salt and water, adjusting the pH to 4.0-10.0, and stirring until the mixture is dissolved to obtain viscoelastic long-carbon-chain amine oxide micelle fracturing fluid resistant to 150 ℃; wherein the mass percentage concentrations of the long-carbon-chain amine oxide thickener, the counter-ion salt and the water in the fracturing fluid are respectively 4-6 percent of the long-carbon-chain amine oxide thickener, 0.8-2.2 percent of the counter-ion salt and the balance of the water.
The molar ratio of the oleamidopropyl dimethyl tertiary amine to the erucamidopropyl dimethyl tertiary amine is preferably 1: 1.
the counter ion salt is selected from: potassium chloride, potassium bromide, sodium salicylate, sodium benzoate, potassium benzoate, and potassium hydrogen phthalate.
The viscoelastic long-carbon-chain amine oxide micelle fracturing fluid prepared by the method has good temperature resistance and shear resistance, and the temperature is 150 ℃ and the shear resistance is 100s-1After 60min of shear, the retained viscosity is higher or close to 30 mPas.
Drawings
FIG. 1 shows a viscoelastic micelle fracturing fluid containing 4 wt% long carbon chain amine oxide and 1 wt% KCl (pH 9) prepared in example 1 of the present invention at 150 deg.C for 100s-1Temperature resistance and shear resistance curve.
FIG. 2 shows a viscoelastic micelle fracturing fluid compounded by 4 wt% long carbon chain amine oxide and 1 wt% KCl (pH 5) prepared in example 2 of the invention at 150 ℃ for 100s-1Temperature resistance and shear resistance curve.
FIG. 3 shows a viscoelastic micelle fracturing fluid compounded by 5 wt% long carbon chain amine oxide and 1 wt% KCl (pH 7) prepared in example 3 of the present invention at 150 deg.C for 100s-1Temperature resistance and shear resistance curve.
Detailed Description
In order to better understand the present invention, the following examples further illustrate the invention, the examples are only used for explaining the invention, not to constitute any limitation of the invention.
Example 1:
6.00g of EDTA.2 Na (Chengdu chemical reagent factory) was weighed and dissolved in 94.00g of tap water, and stirred uniformly to prepare a 6 wt% EDTA.2 Na aqueous solution.
27.88g of anhydrous methanol, 0.82g of 6 wt% EDTA-2 Na aqueous solution and 0.83g of tap water are weighed and added into a three-neck flask provided with a magnetic stirrer and a condenser pipe for uniform stirring; then adding 18.3g of oleamidopropyl dimethyl tertiary amine and 21.1g of erucamidopropyl dimethyl tertiary amine (the total amount of tertiary amine is 0.1mol, the molar ratio is 1: 1), and uniformly stirring; after the temperature is raised to 65 ℃ from the room temperature within 20min, 13.07g of hydrogen peroxide with the mass fraction of 30% (evenly divided into 4 parts, one part is added every 20 minutes) is added within 1 hour, and after stirring reaction is carried out for 5 hours, the long carbon chain amine oxide thickening agent with the solid content of about 50% is obtained.
Weighing 4.00g of long carbon chain amine oxide thickening agent and 0.5g of KCl, adding 45.5g of water, adjusting the pH to 9 by using 0.2mol/L NaOH solution, and stirring at room temperature until the solution is dissolved to obtain the 4 wt% long carbon chain amine oxide +1 wt% KCl (the pH is 9) compound viscoelastic micelle fracturing fluid.
The prepared 4 wt% long carbon chain amine oxide +1 wt% KCl (pH 9) compounded viscoelastic micelle fracturing fluid is at 150 ℃ for 100s-1After shearing for 60min, the retained viscosity is 28.42 mPas, and the temperature and shear resistant curve is shown in figure 1.
Example 2:
the preparation of the long carbon chain amine oxide thickener was the same as in example 1.
Weighing 4.00g of long carbon chain amine oxide thickening agent and 0.5g of KCl, adding 45.5g of water, adjusting the pH to 5 by using 0.1mol/L HCl solution, and stirring at room temperature until the solution is dissolved to obtain the 4 wt% long carbon chain amine oxide +1 wt% KCl (the pH is 5) compound viscoelastic micelle fracturing fluid.
The prepared 4 wt% long carbon chain amine oxide +1 wt% KCl (pH is 5) compounded viscoelastic micelle fracturing fluid is at 150 ℃ for 100s-1After shearing for 60min, the viscosity is kept at 37.72 mPa.s, and the temperature-resistant and shear-resistant curve is shown in FIG. 2.
Example 3:
the preparation of the long carbon chain amine oxide thickener was the same as in example 1.
Weighing 5.00g of long carbon chain amine oxide thickening agent and 0.5g of KCl, adding 44.5g of water, and stirring at room temperature until the mixture is dissolved to obtain the viscoelastic micelle fracturing fluid compounded by 5 wt% of long carbon chain amine oxide and 1 wt% of KCl (pH 7).
The prepared viscoelastic micelle fracturing fluid compounded by 5 wt% of long carbon chain amine oxide and 1 wt% of KCl (pH 7) is at 150 ℃ for 100s-1Shearing for 60min, and maintainingThe retained viscosity was 59.50 mPas, and the temperature and shear resistance curves are shown in FIG. 3.
Claims (3)
1. The viscoelastic long-carbon-chain amine oxide micelle fracturing fluid capable of resisting the temperature of 150 ℃ is characterized by being prepared by the following method, and comprises the following steps:
1) preparing a long-carbon-chain amine oxide thickening agent:
a. mixing 6 wt% disodium ethylene diamine tetraacetate (6 wt% EDTA-2 Na) water solution with anhydrous methanol and water, stirring,
b. b, adding oleamide propyl dimethyl tertiary amine and erucic acid amide propyl dimethyl tertiary amine into the solution prepared in the step a, uniformly stirring, and preparing a mixed tertiary amine solution;
wherein, EDTA-2 Na aqueous solution: anhydrous methanol: water: mass ratio of mixed tertiary amine 1.2%: 40.4%: 1.2%: 57.2 percent, the total mole number of the oleic acid amide propyl dimethyl tertiary amine and the erucic acid amide propyl dimethyl tertiary amine is 0.1 mole, and the mole ratio of the oleic acid amide propyl dimethyl tertiary amine to the erucic acid amide propyl dimethyl tertiary amine is 0: 1-1: 0;
c. adding 30 wt% of hydrogen peroxide into the mixed tertiary amine solution obtained in the step b, wherein the molar ratio of the hydrogen peroxide to the mixed tertiary amine is 1.15:1.0, and oxidizing for 5-7 hours by using the hydrogen peroxide at the temperature of 50-70 ℃ to obtain a long-carbon-chain amine oxide thickening agent;
2) mixing and compounding the long-carbon-chain amine oxide thickening agent, the counter-ion salt and water, adjusting the pH to 4.0-10.0, and stirring until the mixture is dissolved to obtain viscoelastic long-carbon-chain amine oxide micelle fracturing fluid resistant to 150 ℃; wherein the mass percentage concentrations of the long-carbon-chain amine oxide thickener, the counter-ion salt and the water in the fracturing fluid are respectively 4-6 percent of the long-carbon-chain amine oxide thickener, 0.8-2.2 percent of the counter-ion salt and the balance of the water.
2. The viscoelastic long carbon chain amine oxide micellar fracturing fluid resistant to temperatures of 150 ℃ according to claim 1, wherein the molar ratio of oleamidopropyl dimethyl tertiary amine to erucamidopropyl dimethyl tertiary amine is 1: 1.
3. the viscoelastic long carbon chain amine oxide micelle fracturing fluid resistant to temperatures of 150 ℃ according to claim 1, wherein the counter-ion salt is one or more selected from potassium chloride, potassium bromide, sodium salicylate, sodium benzoate, potassium benzoate, and potassium hydrogen phthalate.
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Citations (5)
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|---|---|---|---|---|
| CN101108814A (en) * | 2007-07-24 | 2008-01-23 | 王伟松 | Synthesis method of fatty alkyl dimethyl amine oxide |
| CN104449647A (en) * | 2014-11-25 | 2015-03-25 | 中国石油天然气股份有限公司 | Compound thickening agent for clean fracturing fluid and fracturing fluid as well as preparation method of compound thickening agent |
| CN105567205A (en) * | 2014-10-11 | 2016-05-11 | 中国石油天然气股份有限公司 | Oil displacement agent and synthetic method for docosanamine oxide surfactant |
| CN110257043A (en) * | 2019-07-06 | 2019-09-20 | 西南石油大学 | A kind of stimuli responsive type clean fracturing fluid and preparation method thereof |
| CN111592870A (en) * | 2020-05-25 | 2020-08-28 | 辽宁石油化工大学 | Composite clean fracturing fluid, preparation method and application thereof in oil-gas field fracturing |
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2020
- 2020-12-16 CN CN202011483599.0A patent/CN112480900A/en active Pending
Patent Citations (5)
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|---|---|---|---|---|
| CN101108814A (en) * | 2007-07-24 | 2008-01-23 | 王伟松 | Synthesis method of fatty alkyl dimethyl amine oxide |
| CN105567205A (en) * | 2014-10-11 | 2016-05-11 | 中国石油天然气股份有限公司 | Oil displacement agent and synthetic method for docosanamine oxide surfactant |
| CN104449647A (en) * | 2014-11-25 | 2015-03-25 | 中国石油天然气股份有限公司 | Compound thickening agent for clean fracturing fluid and fracturing fluid as well as preparation method of compound thickening agent |
| CN110257043A (en) * | 2019-07-06 | 2019-09-20 | 西南石油大学 | A kind of stimuli responsive type clean fracturing fluid and preparation method thereof |
| CN111592870A (en) * | 2020-05-25 | 2020-08-28 | 辽宁石油化工大学 | Composite clean fracturing fluid, preparation method and application thereof in oil-gas field fracturing |
Non-Patent Citations (2)
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