CN106268496A - A kind of Shuangzi amphoteric viscoelastic surfactant and preparation method thereof and the clean fracturing fluid with it as thickening agent - Google Patents
A kind of Shuangzi amphoteric viscoelastic surfactant and preparation method thereof and the clean fracturing fluid with it as thickening agent Download PDFInfo
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- CN106268496A CN106268496A CN201610578298.3A CN201610578298A CN106268496A CN 106268496 A CN106268496 A CN 106268496A CN 201610578298 A CN201610578298 A CN 201610578298A CN 106268496 A CN106268496 A CN 106268496A
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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
- C09K8/602—Compositions for stimulating production by acting on the underground formation containing surfactants
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- C—CHEMISTRY; METALLURGY
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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
- C09K8/84—Compositions based on water or polar solvents
- C09K8/86—Compositions based on water or polar solvents containing organic compounds
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Abstract
The present invention proposes a kind of Shuangzi amphoteric viscoelastic surfactant and preparation method thereof and the clean fracturing fluid with it as thickening agent, clean fracturing fluid materials are simple, low cost, microcosmic network structure is obvious, viscoelasticity good, superior, the broken glue of outstanding grittiness is thorough to use the method to prepare, the advantage of its maximum is that temperature tolerance is good, best product shear viscosity below 160 DEG C is not less than 130mPa s, the 25mPa s required much larger than clean fracturing fluid site operation.
Description
Technical field
The present invention relates to oil-gas field development technical field, especially relate to a kind of Shuangzi amphoteric viscoelastic surfactant and
Its preparation method and the clean fracturing fluid with it as thickening agent.
Background technology
The world today, the epoch relying on stratum natural energy to make oil go out from underground gurgle have terminated, global most
Large-scale Thief zone oil gas field comes into the exploitation later stage, and the demand of oil is but persistently being risen by countries in the world, domestic and international oil
The troop of exploration and exploitation starts to march to hypotonic, Oil in Super-low Permeability and unconventional limit oil-gas reservoir, and reservoir fracturing improvement becomes and carries
The key of high oil recovery factor, oil field produces the requirement to reservoir development degree and fracturing reform efficiency and improves constantly, conventional
Reservoir reconstruction (including reforming technology and working solution) exposes all drawbacks, especially with unconventional shale gas, fine and close oil
Deng exploitation, conventional reservoir reconstruction can not meet the requirement of current fracturing reform, and working solution is as " the spirit of reservoir reconstruction
Soul ", its quality decides the success or failure of modification measures, and the research and development of high performance operation liquid become current unconventionaloil pool Tibetan reservoir and change
Make middle problem demanding prompt solution.
Schlumberger in 1997, by viscoelastic surfactant fracturing fluid successful Application in reservoir fracturing improvement, starts
The research boom of clean fracturing fluid, oil and gas reservoir High Efficiency Reform low-grade to the world provide possibility.This fracturing fluid is with often
The difference of rule polymer fracturing fluid maximum is, it belongs to structural fluid, is shown as typical elastic fluid in a shear condition,
There is under low viscosity good prop-carrying capacity, broken natural or man-made polymer's fracturing fluid dependence fluid viscosity suspended prop
Normal mode, thus be conducive to the formation in long crack at a low viscosity, and breaking glue solution without residue, there is cleaning crack wall
Effect, fracture condudtiviy can be effectively improved, thus receive the extensive concern of oilfield.
But, due to surfactant unstability under the conditions of high temperature, high salt etc., and its side such as consumption, cost
The reason in face, clean fracturing fluid application in reservoir reconstruction receives serious restriction.It is prominent that current clean fracturing fluid exists
Ging wrong and have: (1) use cost is high, the viscoelastic surfactant that the clean fracturing fluid reported such as current document uses is biography
The single tail surface active agent of system, its critical micelle concentration is higher, and in actual application, consumption is too big, and cost is high;(2) according to the literature,
Applicable formation temperature is generally less than 120 DEG C, and existing clean fracturing fluid technology cannot be applied on the stratum of higher temperature;(3) by force
The ability of poor stability in electrolyte, the especially metal ion of resistance to divalent is lower, is susceptible to saponification or salt in concentrated water
Analysis phenomenon, causes clean fracturing fluid to use.
Summary of the invention
The present invention proposes a kind of Shuangzi amphoteric viscoelastic surfactant and preparation method thereof and clear with it as thickening agent
Clean fracturing fluid, can solve that existing clean fracturing liquid system exists temperature tolerance is poor, cost height, the problem of complicated process of preparation.
A kind of technical scheme of the present invention is achieved in that a kind of Shuangzi amphoteric viscoelastic surfactant, and it has
Following general structure:
Wherein R is the aliphatic unsaturated hydrocarbon of carbon number 18-21.
The another kind of technical scheme of the present invention is achieved in that the preparation of a kind of Shuangzi amphoteric viscoelastic surfactant
Method, comprises the following steps:
(1) by the 2 of 10mmol, 2 pairs of (bromomethyl)-1,3-PDs join in round-bottomed flask, are molten with oxolane
Agent, adds the fatty acid amide propyl dimethylamine of 20mmol, and 60 DEG C are refluxed 12 hours, wherein n (2,2 pairs of (bromomethyl)-1,3-third
Glycol): n (fatty acid amide propyl dimethylamine)=1:2, after reaction terminates, decompression distillation obtains intermediate A;
(2) the intermediate A oxolane first step obtained dissolves, and adds the sodium hydride of 20~22mmol, and room temperature stirs
Mix about 15min, after then being dissolved with 50mL oxolane by the PS of 20mmol, be slowly dropped to intermediate
In the solution of A and sodium hydride reaction, 60 DEG C are refluxed 12 hours, and wherein n (intermediate A): n (sodium hydride): n is (in 1,3-propane sulphur
Ester)=1:2~2.2:2, to react and react with unnecessary sodium hydride with hydrochloric acid after terminating, distillation of reducing pressure after filtration obtains clear yellow viscous
Gluey Shuangzi amphoteric viscoelastic surfactant.
As the preferred technical scheme of one, in course of reaction, mole dosage of sodium hydride should be the 2~2.2 of intermediate A
Times.
As the preferred technical scheme of one, described fatty acid is stearic acid, oleic acid, arachidic acid or erucic acid.
The another kind of technical scheme of the present invention is achieved in that a kind of application Shuangzi amphoteric viscoelastic surfactant is
The clean fracturing fluid of thickening agent, includes according to mass fraction: 1.8~the viscoelastic surfactant of 4.3%, 0.8~1.1%
Counter ion salt or inorganic salt, the water composition of surplus.
As the preferred technical scheme of one, described counter ion or inorganic salt include potassium chloride, ammonium chloride, sodium salicylate,
One or more the mixing therein of sodium benzoate, benzoic acid hydrogen potassium, carboxyl benzene sulfonate and sulfosalicylic acid sodium salt.
As the preferred technical scheme of one, it is 1.4~4.3% that the preparation of described clean fracturing fluid only needs mass fraction
Viscoelastic surfactant join dissolved with mass fraction be 0.8~1.1% counter ion salt aqueous solution in, stirring to the most molten
Solve.
The invention provides a kind of method utilizing fatty acid to prepare Shuangzi amphoteric salt viscoelastic surfactant, Yi Jili
The method preparing clean fracturing fluid with this viscoelastic surfactant, prepared clean fracturing fluid can be protected below 160 DEG C
Hold the viscoelasticity of excellence, can be used for the fracturing fluid storey increase design of middle low permeability reservoir.
Have employed technique scheme, the invention have the benefit that
(1) preparation method of thickening agent is simple, and product yield is high, generally reaches more than 98%, and impurity is few, to properties of product
Impact smaller.
(2) consumption is few, low cost, and the critical micelle concentration of viscoelastic surfactant prepared by employing said method is 2
~3 × 10-4Mol/L, 1~2 order of magnitude lower than routine list tail viscoelastic surfactant.
(3) temperature tolerance is good, and existing clean fracturing fluid temperature tolerance is generally less than 120 DEG C, and only only a few clean fracturing fluid leads to
Crossing interpolation auxiliary agent and can be only achieved 135 DEG C, the composition causing system is more complicated, and cost increases, the optimal cleaning that the present invention provides
Fracturing fluid is at 159 DEG C, 170s-1Under the conditions of shear 1 hour, viscosity is maintained at more than 130mPa s, have excellence viscoelasticity.
(4) clean fracturing fluid preparation is simple, it is only necessary to the thickening agent of required quality joins certain density counter ion salt
In aqueous solution, stirring is to dissolving.
Accompanying drawing explanation
In order to be illustrated more clearly that the embodiment of the present invention or technical scheme of the prior art, below will be to embodiment or existing
In having technology to describe, the required accompanying drawing used is briefly described, it should be apparent that, the accompanying drawing in describing below is only this
Some embodiments of invention, for those of ordinary skill in the art, on the premise of not paying creative work, also may be used
To obtain other accompanying drawing according to these accompanying drawings.
Fig. 1 is the rheological curve of the clean fracturing fluid in embodiment one with 4.3% thickening agent+1.1%KCl preparation
Fig. 2 is the rheological curve of the clean fracturing fluid in embodiment one with 1.8% thickening agent+0.8%KCl preparation
Fig. 3 is the rheological curve of the clean fracturing fluid in embodiment two with 4.3% thickening agent+1.1%KCl preparation
Fig. 4 is the rheological curve of the clean fracturing fluid in embodiment two with 1.8% thickening agent+0.8%KCl preparation
Fig. 5 is the rheological curve of the clean fracturing fluid in embodiment three with 4.3% thickening agent+1.1%KCl preparation
Fig. 6 is the rheological curve of the clean fracturing fluid in embodiment three with 1.8% thickening agent+0.8%KCl preparation
Fig. 7 is the rheological curve of the clean fracturing fluid in embodiment four with 4.3% thickening agent+1.1%KCl preparation
Fig. 8 is the rheological curve of the clean fracturing fluid in embodiment four with 1.8% thickening agent+0.8%KCl preparation
Detailed description of the invention
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clear, complete
Describe, it is clear that described embodiment is only a part of embodiment of the present invention rather than whole embodiments wholely.Based on
Embodiment in the present invention, it is every other that those of ordinary skill in the art are obtained under not making creative work premise
Embodiment, broadly falls into the scope of protection of the invention.
A kind of Shuangzi amphoteric viscoelastic surfactant, it has a following general structure:
Wherein R is the aliphatic unsaturated hydrocarbon of carbon number 18-21.
Embodiment one:
By the 2 of 10mmol, 2 pairs of (bromomethyl)-1,3-PDs join in round-bottomed flask, with oxolane as solvent,
Adding the erucyl amide diemethylamine of 20mmol, 60 DEG C are refluxed 12 hours, wherein n (2,2 pairs of (bromomethyl)-1,3-the third two
Alcohol): n (erucyl amide diemethylamine)=1:2, after reaction terminates, decompression distillation obtains intermediate A.During the first step is obtained
Mesosome A oxolane dissolves, and adds the sodium hydride of 20~22mmol, about stirring at normal temperature 15min, then by the 1 of 20mmol,
After the oxolane of 3 propane sultone 50mL dissolves, it is slowly dropped in the solution of intermediate A and sodium hydride reaction, 60 DEG C
Refluxing 12 hours, wherein n (intermediate A): n (sodium hydride): n (1,3 propane sultone)=1:2~2.2:2, reaction is used after terminating
Hydrochloric acid reacts with unnecessary sodium hydride, and distillation of reducing pressure after filtration obtains clear yellow viscous glue Shuangzi both sexes Viscoelastic surfactant
Agent.The critical micelle concentration of the surfactant obtained is 3.63 × 10-4Mol/L, 4.3% thickening agent+1.1%KCl and 1.8%
The clean fracturing fluid of thickening agent+0.8%KCl preparation is respectively at 159 DEG C, 170s-1With 119 DEG C, 170s-1Rheological characteristic such as accompanying drawing 1
Shown in accompanying drawing 2, static outstanding sand is 0 without substantially sedimentation by 30% kerosene breaking glue solution viscosity after breaking gel in 2 hours.
Embodiment two:
By the 2 of 10mmol, 2 pairs of (bromomethyl)-1,3-PDs join in round-bottomed flask, with oxolane as solvent,
Adding the arachidamide diemethylamine of 20mmol, 60 DEG C are refluxed 12 hours, wherein n (2,2 pairs of (bromomethyl)-1,3-the third two
Alcohol): n (arachidamide diemethylamine)=1:2, after reaction terminates, decompression distillation obtains intermediate A.The first step is obtained
Intermediate A oxolane dissolves, and adds the sodium hydride of 20~22mmol, about stirring at normal temperature 15min, then by 20mmol's
After the oxolane of 1,3 propane sultone 50mL dissolves, it is slowly dropped in the solution of intermediate A and sodium hydride reaction, 60
DEG C backflow 12 hours, wherein n (intermediate A): n (sodium hydride): n (1,3 propane sultone)=1:2~2.2:2, reaction terminate after
Reacting with unnecessary sodium hydride with hydrochloric acid, distillation of reducing pressure after filtration obtains clear yellow viscous glue Shuangzi both sexes Viscoelastic surfactant
Agent.The critical micelle concentration of the surfactant obtained is 3.63 × 10-4Mol/L, 4.3% thickening agent+1.1% sodium salicylate and
The clean fracturing fluid of 1.8% thickening agent+0.8% sodium salicylate preparation is respectively at 159 DEG C, 170s-1With 119 DEG C, 170s-1Stream
Degeneration is as shown in accompanying drawing 3 and accompanying drawing 4, and static outstanding sand 2 hours without substantially sedimentation by 30% kerosene breaking glue solution viscosity is after breaking gel
0。
Embodiment three:
By the 2 of 10mmol, 2 pairs of (bromomethyl)-1,3-PDs join in round-bottomed flask, with oxolane as solvent,
Adding the oleamide diemethylamine of 20mmol, 60 DEG C are refluxed 12 hours, wherein n (2,2 pairs of (bromomethyl)-1,3-the third two
Alcohol): n (oleamide diemethylamine)=1:2, after reaction terminates, decompression distillation obtains intermediate A.During the first step is obtained
Mesosome A oxolane dissolves, and adds the sodium hydride of 20~22mmol, about stirring at normal temperature 15min, then by the 1 of 20mmol,
After the oxolane of 3 propane sultone 50mL dissolves, it is slowly dropped in the solution of intermediate A and sodium hydride reaction, 60 DEG C
Refluxing 12 hours, wherein n (intermediate A): n (sodium hydride): n (1,3 propane sultone)=1:2~2.2:2, reaction is used after terminating
Hydrochloric acid reacts with unnecessary sodium hydride, and distillation of reducing pressure after filtration obtains clear yellow viscous glue Shuangzi both sexes Viscoelastic surfactant
Agent.The critical micelle concentration of the surfactant obtained is 3.63 × 10-4Mol/L, 4.3% thickening agent+0.8%KCl and 1.8%
The clean fracturing fluid of thickening agent+1.1% sodium salicylate preparation is respectively at 159 DEG C, 170s-1With 119 DEG C, 170s-1Rheological characteristic such as
Shown in accompanying drawing 5 and accompanying drawing 6, static outstanding sand is 0 without substantially sedimentation by 30% kerosene breaking glue solution viscosity after breaking gel in 2 hours.
Embodiment four:
By the 2 of 10mmol, 2 pairs of (bromomethyl)-1,3-PDs join in round-bottomed flask, with oxolane as solvent,
Adding the stearic amide diemethylamine of 20mmol, 60 DEG C are refluxed 12 hours, wherein n (2,2 pairs of (bromomethyl)-1,3-the third two
Alcohol): n (stearic amide diemethylamine)=1:2, after reaction terminates, decompression distillation obtains intermediate A.The first step is obtained
Intermediate A oxolane dissolves, and adds the sodium hydride of 20~22mmol, about stirring at normal temperature 15min, then by 20mmol's
After the oxolane of 1,3 propane sultone 50mL dissolves, it is slowly dropped in the solution of intermediate A and sodium hydride reaction, 60
DEG C backflow 12 hours, wherein n (intermediate A): n (sodium hydride): n (1,3 propane sultone)=1:2~2.2:2, reaction terminate after
Reacting with unnecessary sodium hydride with hydrochloric acid, distillation of reducing pressure after filtration obtains clear yellow viscous glue Shuangzi both sexes Viscoelastic surfactant
Agent.The critical micelle concentration of the surfactant obtained is 3.63 × 10-4Mol/L, 4.0% thickening agent+1.0% sodium salicylate and
The clean fracturing fluid of 2.2% thickening agent+0.8%KCl preparation is respectively at 159 DEG C, 170s-1With 119 DEG C, 170s-1Rheological characteristic such as
Shown in accompanying drawing 7 and accompanying drawing 8, static outstanding sand is 0 without substantially sedimentation by 30% kerosene breaking glue solution viscosity after breaking gel in 2 hours.
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all essences in the present invention
Within god and principle, any modification, equivalent substitution and improvement etc. made, should be included within the scope of the present invention.
Claims (7)
1. a Shuangzi amphoteric viscoelastic surfactant, it is characterised in that it has a following general structure:
Wherein R is the aliphatic unsaturated hydrocarbon of carbon number 18-21.
2. the preparation method of a Shuangzi amphoteric viscoelastic surfactant, it is characterised in that comprise the following steps:
(1) by the 2 of 10mmol, 2 pairs of (bromomethyl)-1,3-PDs join in round-bottomed flask, with oxolane as solvent, add
Entering the fatty acid amide propyl dimethylamine of 20mmol, 60 DEG C are refluxed 12 hours, wherein n (2,2 pairs of (bromomethyl)-1,3-the third two
Alcohol): n (fatty acid amide propyl dimethylamine)=1:2, after reaction terminates, decompression distillation obtains intermediate A;
(2) the intermediate A oxolane first step obtained dissolves, and adds the sodium hydride of 20~22mmol, stirring at normal temperature
About 15min, after then being dissolved with 50mL oxolane by the PS of 20mmol, is slowly dropped to intermediate A
With in the solution of sodium hydride reaction, 60 DEG C are refluxed 12 hours, and wherein n (intermediate A): n (sodium hydride): n is (in 1,3-propane sulphur
Ester)=1:2~2.2:2, to react and react with unnecessary sodium hydride with hydrochloric acid after terminating, distillation of reducing pressure after filtration obtains clear yellow viscous
Gluey Shuangzi amphoteric viscoelastic surfactant.
The preparation method of a kind of Shuangzi amphoteric viscoelastic surfactant the most as claimed in claim 2, it is characterised in that reaction
During mole dosage is intermediate A 2~2.2 times of sodium hydride.
The preparation method of a kind of Shuangzi amphoteric viscoelastic surfactant the most as claimed in claim 2, described fatty acid is hard
Fat acid, oleic acid, arachidic acid or erucic acid.
5. applying Shuangzi amphoteric viscoelastic surfactant described in claim 1 is a clean fracturing fluid for thickening agent, and it is special
Levy and be, include according to mass fraction: 1.8~the viscoelastic surfactant of 4.3%, 0.8~the counter ion salt of 1.1% or nothing
Machine salt, the water composition of surplus.
6. clean fracturing fluid as claimed in claim 5, it is characterised in that described counter ion or inorganic salt include potassium chloride, chlorine
One or more in change ammonium, sodium salicylate, sodium benzoate, benzoic acid hydrogen potassium, carboxyl benzene sulfonate and sulfosalicylic acid sodium salt
Mixing.
7. clean fracturing fluid as claimed in claim 5, it is characterised in that the preparation of described clean fracturing fluid only needs to divide quality
Number be 1.8~4.3% viscoelastic surfactant join mass fraction be 0.8~1.1% counter ion saline solution in,
Stirring is to being completely dissolved.
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CN108047078A (en) * | 2018-01-11 | 2018-05-18 | 西南石油大学 | Three sub- cationic viscoelastic surfactants and preparation method thereof, application and clean fracturing fluid |
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