CN101481608B - Clean fracturing fluid and use thereof - Google Patents
Clean fracturing fluid and use thereof Download PDFInfo
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- CN101481608B CN101481608B CN200910013666XA CN200910013666A CN101481608B CN 101481608 B CN101481608 B CN 101481608B CN 200910013666X A CN200910013666X A CN 200910013666XA CN 200910013666 A CN200910013666 A CN 200910013666A CN 101481608 B CN101481608 B CN 101481608B
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Abstract
The invention relates to a clean fracturing fluid and the application thereof, and the fracturing fluid comprises the components based on the parts by mass: 50-80 parts of thickening agent, 10-35 parts of salicylate and 2-5 parts of gel breaker. The clean fracturing fluid is used for fracturing oil field; in the application site, the components are mixed according to the parts by mass to prepare aqueous solution with the mass percent of 2-6% and evenly stirred, and then is thrown into an oil well together fracturing propping agent. The fracturing propping agent of the clean fracturing fluid is even in dispersion and thorough in gelout.
Description
(1) technical field
The present invention relates to be used in a kind of oilfield exploitation procedure the fracturing liquid and the preparation method of fracturing yield increasing measure, be specifically related to a kind of clean fracturing fluid and preparation method thereof, belong to the oilfield chemical technology field.
(2) background technology
The oil recovery rate and the recovery percent of reserves of China's oil field low-permeability oil deposit are all lower at present, and the stable yields difficulty is very big, and fracturing technology is the dominant technology of volume increase.The most normal fracturing liquid that uses is the aqueous-based polymers fracturing liquid both at home and abroad, and natural or synthetic polymer forms full-bodied fracturing liquid under the effect of linking agent.The shortcoming of these fracturing liquid systems is that fracturing liquid rubber-breaking is incomplete, and residue will remain in the crack behind the broken glue, will seriously reduce the rate of permeation of proppant pack, thereby the injury payzone causes the fracturing effect variation.A kind of novel clean fracturing fluid technology-viscoelasticity tensio-active agent fracturing liquid technology, aspect oil reservoir, fissured injury and raising fracturing reform effect, has special advantages in reduction, this of the fracturing fluid thickening material is a tensio-active agent, there is not polymkeric substance in the system, residue is few behind the broken glue, injury to the stratum is little, is specially adapted to the fracturing reform of low-permeability oil deposit.
U.S. Pat 5551516 discloses the of the fracturing fluid composition of viscoelasticity tensio-active agent, contains N-mustard oil base-N of at least 60%, and N-dihydroxy ethyl ammonio methacrylate adds Repone K or ammonium chloride and sodium salicylate simultaneously.
Chinese patent ZL200310116815.8 (Granted publication CN1285700C) discloses a kind of prescription of clean fracturing fluid, is mixed by the unsaturated fatty acid salt of 18 carbon atoms and lipid acid, mineral alkali and the salt solution of salt solution mixing or 18 carbon atoms.
Chinese patent ZL03110938.1 (Granted publication CN1206307C) discloses the non-injury fracturing fluid of being made up of cetyl trimethylammonium bromide, sodium salicylate, water.
Chinese patent ZL200410078253.7 (Granted publication CN1313563C) discloses a kind of clean fracturing solution additive: long alkyl chain length quaternary ammonium salt, long alkyl chain length dimethyl oxidation amine, salicylate, glycol ether, low-carbon alcohol, water.
Chinese patent 200810150252.7 (publication number CN101298555A) has been applied for a kind of harmless clean fracturing fluid, comprises quaternary ammonium alkyl salt mixture, gegenion salt, low-carbon (LC) alcohol and water.
Prior art is applied to the oil field compression fracture volume increase, show than the of the fracturing fluid advantage of aqueous-based polymers in construction and prevent aspect the formation damage etc., all adopt fracturing liquid to contact the back with underground crude oil and realize broken glue, but at gas well and low oil well, the fracturing liquid in high sand ratio stage of oil saturation, fracturing liquid fails fully to contact with underground crude oil, be difficult to thoroughly broken glue, occur returning discharge opeing viscosity higher, return the phenomenon that discharge opeing contains sand sometimes; And there is a problem that of the fracturing fluid rate of crosslinking is fast, propping agent is easily united.
(3) summary of the invention
At the deficiencies in the prior art, the present invention proposes a kind of clean fracturing fluid that can not rely on the broken glue of resident fluid (crude oil, water) and preparation method thereof, and broken glue is thorough, and the breaking glue solution viscosity is low, and of the fracturing fluid rate of crosslinking can postpone, propping agent is not united.
Clean fracturing fluid of the present invention, as follows by the mass parts component:
Thickening material 50-80 part, salicylate 10-35 part, gel breaker 2-5 part.
Preferably, described thickening material N-fatty amide propyl-N-(1,2 hydroxypropyl)-N, N-alkyl dimethyl ammonium chloride or N-fatty amide propyl-N-hydroxyethyl-N, N-alkyl dimethyl ammonium chloride.
Preferably, described salicylate is sodium salicylate or potassium salicylate.
Preferably, described gel breaker is Potassium Persulphate, ammonium persulphate, potassium bromate, potassium permanganate, three oxygen methylbenzene or benzyl chlorides, perhaps the capsule that forms through coating of Potassium Persulphate, ammonium persulphate, potassium bromate, potassium permanganate, three oxygen methylbenzene or benzyl chloride.
Preferably, described thickening material is to make by the following method:
(1) in synthesis reaction vessel, quantitatively adds lipid acid or fatty acid ester.Need be heated to fusing fully when using solid material.
(2) in above-mentioned synthesis reaction vessel, slowly add N, N-dimethylated propyl diethylenetriamine, lipid acid or fatty acid ester and N, the mol ratio of N-dimethylated propyl diethylenetriamine 1: 1.1, the limit edged stirs, and keeps temperature to be lower than 90 ℃, be warming up to 150-180 ℃ after adding, and under this temperature, react about 5-7hr.Keep vacuum tightness 0.2-1MPa in the reaction process, timing sampling, the amine value with hydrochloric acid standard solution mensuration mixture is terminal point when the amine value of reactant no longer changes.When reaction raw materials is fatty acid ester, add the KOH of reaction-ure mixture 0.5% in the synthesis reaction vessel as catalyzer.
When (3) reducing to the temperature in the above-mentioned still below 60 ℃, add ethanol, dosage is reactant gross weight 15-40%, after stirring, add halogenated hydroxyl alcohol, the mol ratio of lipid acid or fatty acid ester and halogenated hydroxyl alcohol 1: 1.2, the pH value of the NaOH aqueous solution conditioned reaction thing of usefulness 20%wt is between 7-8.Be warming up to 80 ℃ ± 5 ℃ again, back flow reaction 4-6hr gets product.
One of the preferred oleic acid of the described lipid acid of above-mentioned steps (1) or sinapinic acid or its combination.
The described fatty acid ester preferred plant of above-mentioned steps (1) grease, fatty acid methyl ester or fatty-acid ethyl ester.
Described Vegetable oil lipoprotein is Oleum Gossypii semen, peanut oil, oleum lini or rape seed oil.
Described fatty acid methyl ester is the methyl esters of oleic acid or sinapinic acid, and described fatty-acid ethyl ester is the ethyl ester of oleic acid or sinapinic acid.
The preferred 3-chloro-1 of the described halogenated hydroxyl alcohol of above-mentioned steps (3), 2-propylene glycol or ethylene chlorhydrin.
The application of clean fracturing fluid of the present invention is used for the oil field compression fracture volume increase.Concrete using method is:
After site of deployment is mixed each component by mass parts, be made into the aqueous solution of 1-6% mass percent, stir, squeeze into the down-hole with fracturing propping agents then.According to field requirement, also can add Repone K.Fracturing propping agents are by state of the art.
Clean fracturing fluid of the present invention has following excellent results:
1, the thickening material that adopts in the clean fracturing fluid of the present invention has the following advantages: the A good fluidity, and viscosity is lower than 100mPaS under the normal temperature; B disperses in water easily, stirs a little during preparation or rocks and can dissolve fully; C concentration height has reduced the transportation burden.
2, clean fracturing fluid crosslinking time of the present invention is adjustable.
3, the broken glue of clean fracturing fluid of the present invention is thorough, does not contact with crude oil, local water, and the breaking glue solution viscosity is less than 5mPaS.
4, clean fracturing fluid of the present invention, propping agent is uniformly dispersed, and does not unite.
5, clean fracturing fluid of the present invention is in process for preparation, even vigorous agitation, also non-foam, convenient construction.
6, clean fracturing fluid breaking glue solution table of the present invention, interfacial tension are low, are easy to the row of returning.
(4) embodiment
Following examples only are used to further specify the present invention, but do not limit the present invention.
Embodiment 1, thickening material N-amine hydroxybenzene propyl group-N-(1,2 hydroxyl-propyl group)-N, N-alkyl dimethyl ammonium chloride synthetic
In the 1000L synthesis reactor, add 460Kg oleic acid, add 183Kg N then, the N-dimethylated propyl diethylenetriamine, the limit edged stirs, and is warming up to 150 ℃ ± 5 ℃ after adding, about reaction 6hr, timing sampling in the reaction process, amine value with hydrochloric acid standard solution mensuration mixture when the amine value of reactant no longer changes, is cooled to 60 ℃, add 20Kg ethanol, stir.Add 232Kg 3-chloro-1, the 2-propylene glycol, the pH value of the NaOH aqueous solution conditioned reaction thing with 20% is warming up to 80 ℃ ± 5 ℃ between 7-8, and back flow reaction 5hr promptly gets product N-amine hydroxybenzene propyl group-N-(1,2 hydroxyl-propyl group)-N, N-alkyl dimethyl ammonium chloride.
Embodiment 2, thickening material N-mustard seed amido propyl-N-(1,2 hydroxyl-propyl group)-N, N-alkyl dimethyl ammonium chloride synthetic
In the 1000L synthesis reactor, add the 414Kg sinapinic acid, add 207Kg N then, the N-dimethylated propyl diethylenetriamine, the limit edged stirs, and is warming up to 160 ℃ ± 5 ℃ after adding, about reaction 6hr, timing sampling in the reaction process, amine value with hydrochloric acid standard solution mensuration mixture when the amine value of reactant no longer changes, is cooled to 60 ℃, add 21Kg ethanol, stir.Add 263Kg 3-chloro-1, the 2-propylene glycol, the pH value of the NaOH aqueous solution conditioned reaction thing with 20% is warming up to 80 ℃ ± 5 ℃ between 7-8, and back flow reaction 5hr promptly gets product N-mustard seed amido propyl-N-(1,2 hydroxyl-propyl group)-N, N-alkyl dimethyl ammonium chloride.
Embodiment 3, thickening material N-mustard seed amido propyl-N-(1,2 hydroxyl-propyl group)-N, N-alkyl dimethyl ammonium chloride synthetic
In the 1000L synthesis reactor, add 440Kg sinapinic acid methyl esters, add 207Kg N then, the N-dimethylated propyl diethylenetriamine, the limit edged stirs, and adds the back and adds 3.3Kg KOH as catalyzer, be warming up to 160 ℃ ± 5 ℃, about reaction 6hr, timing sampling in the reaction process is with the amine value of hydrochloric acid standard solution mensuration mixture, when the amine value of reactant no longer changes, be cooled to 60 ℃, add 21Kg ethanol, stir.Add 263Kg 3-chloro-1, the 2-propylene glycol, the pH value of the NaOH aqueous solution conditioned reaction thing with 20% is warming up to 80 ℃ ± 5 ℃ between 7-8, and back flow reaction 5hr promptly gets product.
Embodiment 4, thickening material N-amine hydroxybenzene propyl group-N-hydroxyethyl-N, N-alkyl dimethyl ammonium chloride synthetic
In the 1000L synthesis reactor, add 460Kg oleic acid, add 183Kg N then, the N-dimethylated propyl diethylenetriamine, the limit edged stirs, and is warming up to 150 ℃ ± 5 ℃ after adding, about back flow reaction 6hr, timing sampling in the reaction process, amine value with hydrochloric acid standard solution mensuration mixture when the amine value of reactant no longer changes, is cooled to 60 ℃, add 20Kg ethanol, stir.Add the 157Kg ethylene chlorhydrin, the pH value of the NaOH aqueous solution conditioned reaction thing with 20% is warming up to 80 ℃ ± 5 ℃ between 7-8, and back flow reaction 5hr promptly gets product N-amine hydroxybenzene propyl group-N-hydroxyethyl-N, N-alkyl dimethyl ammonium chloride.
Embodiment 5, clean fracturing fluid
Press mass parts: 65 parts of thickening materials, 32 parts of sodium salicylates, 3 parts of Potassium Persulphates.Used thickening material is embodiment 2 synthetic.
With being made into the aqueous solution of 4% mass percent after the above each component mixing, stir crosslinking time 2min, 100 ℃, 170S
-1After shearing 1hr, viscosity 120mPaS, fracturing propping agents are uniformly dispersed.Residue is 0 behind the broken glue, breaking glue solution viscosity 5mPaS, surface tension 25mN/m, interfacial tension 1.2mN/m.
Embodiment 6, clean fracturing fluid
As embodiment 5, different is that gel breaker is an ammonium persulphate.Product performance are constant.
Embodiment 7, clean fracturing fluid
As embodiment 4, different is that salicylate is a potassium salicylate.Product performance are constant.
Embodiment 8, clean fracturing fluid
Press mass parts: 60 parts of thickening materials, 35 parts of sodium salicylates, 5 parts of Potassium Persulphates.Thickening material is embodiment 1 synthetic.
With being made into the aqueous solution of 5% mass percent after the above each component mixing, stir crosslinking time 1.8min, 80 ℃, 170S
-1After shearing 1hr, be viscosity 90mPaS.
Embodiment 9, clean fracturing fluid
As embodiment 5, different is that thickening material is embodiment 1 synthetic.The aqueous solution that is made into 4% mass percent stirs, crosslinking time 1.8min, 80 ℃, 170S
-1After shearing 1hr, viscosity 80mPaS.
Embodiment 10, clean fracturing fluid
As embodiment 5, different is that thickening material is embodiment 3 synthetic.Product performance are identical with embodiment 4.Embodiment 11, clean fracturing fluid
As embodiment 8, different is that thickening material is embodiment 4 synthetic.Product performance are identical with embodiment 8.
Claims (5)
1. clean fracturing fluid is characterized in that by the mass parts component as follows:
Thickening material 50-80 part, salicylate 10-35 part, gel breaker 2-5 part;
Described thickening material is N-fatty amide propyl-N-(1,2 hydroxypropyl)-N, N-alkyl dimethyl ammonium chloride or N-fatty amide propyl-N-hydroxyethyl-N, N-alkyl dimethyl ammonium chloride;
Described gel breaker is Potassium Persulphate, ammonium persulphate, potassium bromate, potassium permanganate, three oxygen methylbenzene or benzyl chlorides, perhaps the capsule that forms through coating of Potassium Persulphate, ammonium persulphate, potassium bromate, potassium permanganate, three oxygen methylbenzene or benzyl chloride;
After site of deployment is mixed each component by mass parts, be made into the aqueous solution of 1-6% mass percent, stir, squeeze into the down-hole with fracturing propping agents then.
2. clean fracturing fluid as claimed in claim 1 is characterized in that described salicylate is selected from sodium salicylate or potassium salicylate.
3. clean fracturing fluid as claimed in claim 1 is characterized in that described thickening material is to make by the following method:
(1) in synthesis reaction vessel, quantitatively adds lipid acid or fatty acid ester; Need be heated to fusing fully when using solid material;
(2) in above-mentioned synthesis reaction vessel, slowly add N, N-dimethylated propyl diethylenetriamine, lipid acid or fatty acid ester and N, the mol ratio of N-dimethylated propyl diethylenetriamine 1: 1.1, the limit edged stirs, and keeps temperature to be lower than 90 ℃, be warming up to 150-180 ℃ after adding, and under this temperature, react about 5-7hr; Keep vacuum tightness 0.2-1MPa in the reaction process, timing sampling, the amine value with hydrochloric acid standard solution mensuration mixture is terminal point when the amine value of reactant no longer changes; When reaction raw materials is fatty acid ester, add the KOH of reaction-ure mixture 0.5% in the synthesis reaction vessel as catalyzer;
When (3) reducing to the temperature in the above-mentioned still below 60 ℃, add ethanol, dosage is reactant gross weight 15-40%, after stirring, add halogenated hydroxyl alcohol, described halogenated hydroxyl alcohol is 3-chloro-1,2-propylene glycol or ethylene chlorhydrin, the mol ratio of lipid acid or fatty acid ester and halogenated hydroxyl alcohol 1: 1.2, the pH value of the NaOH aqueous solution conditioned reaction thing of usefulness 20wt% is between 7-8; Be warming up to 80 ℃ ± 5 ℃ again, back flow reaction 4-6hr gets product.
4. clean fracturing fluid as claimed in claim 3 is characterized in that the described lipid acid of step (1) is one of oleic acid or sinapinic acid or its combination.
5. clean fracturing fluid as claimed in claim 3 is characterized in that the described fatty acid ester of step (1) is Vegetable oil lipoprotein, fatty acid methyl ester or fatty-acid ethyl ester; Wherein, described Vegetable oil lipoprotein is Oleum Gossypii semen, peanut oil or rape seed oil, and described fatty acid methyl ester is the methyl esters of oleic acid or sinapinic acid, and described fatty-acid ethyl ester is the ethyl ester of oleic acid or sinapinic acid.
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| CN200910013666XA CN101481608B (en) | 2009-01-19 | 2009-01-19 | Clean fracturing fluid and use thereof |
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| CN200910013666XA CN101481608B (en) | 2009-01-19 | 2009-01-19 | Clean fracturing fluid and use thereof |
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| CN101481608A CN101481608A (en) | 2009-07-15 |
| CN101481608B true CN101481608B (en) | 2011-08-10 |
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| CN102010704B (en) * | 2010-11-18 | 2012-11-07 | 陕西延长石油(集团)有限责任公司研究院 | Viscoelastic surfactant cleaning fracturing fluid gel breaker and field construction method |
| CN102155209B (en) * | 2011-01-21 | 2014-01-01 | 中国石油大学(北京) | Method for fracturing stratum by acidity viscoelastic fluid |
| CN102643637B (en) * | 2012-03-22 | 2013-10-16 | 中国石油天然气股份有限公司 | Clear fracturing fluid |
| US8424784B1 (en) * | 2012-07-27 | 2013-04-23 | MBJ Water Partners | Fracture water treatment method and system |
| AU2014251274B2 (en) * | 2013-04-08 | 2017-12-21 | Expansion Energy, Llc | Non-hydraulic fracturing and cold foam proppant delivery systems, methods, and processes |
| CN103265937B (en) * | 2013-05-07 | 2015-10-28 | 四川省博仁达石油科技有限公司 | Be applicable to the of the fracturing fluid gel breaker of class A foam A |
| CN103468237A (en) * | 2013-06-13 | 2013-12-25 | 中国石油集团西部钻探工程有限公司 | Clean fracturing fluid and preparation method thereof |
| CN103421473A (en) * | 2013-08-02 | 2013-12-04 | 中国石油天然气集团公司 | Emulsifier for novel high-temperature water-in-oil drilling fluid |
| CN103980876B (en) * | 2014-05-22 | 2016-08-17 | 西安石油大学 | Applicable clean fracturing fluid constructed at low ambient temperatures and preparation method thereof |
| CN105199704A (en) * | 2015-10-15 | 2015-12-30 | 中国石油集团川庆钻探工程有限公司长庆井下技术作业公司 | Gel breaker for clean fracturing fluid and application method of gel breaker |
| CN106644818B (en) * | 2016-12-29 | 2023-03-31 | 重庆科技学院 | Shale gas well yield simulation tester under slippery water effect |
| CN111234796A (en) * | 2020-01-21 | 2020-06-05 | 中国石油天然气股份有限公司 | Surfactant and preparation method thereof |
| CN115011326A (en) * | 2022-07-22 | 2022-09-06 | 山东欣广化学有限公司 | Clean fracturing fluid for oil field and preparation method thereof |
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