CN106268496B - A kind of Shuangzi amphoteric viscoelastic surfactant and preparation method thereof and using it as the clean fracturing fluid of thickening agent - Google Patents
A kind of Shuangzi amphoteric viscoelastic surfactant and preparation method thereof and using it as the clean fracturing fluid of thickening agent Download PDFInfo
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- CN106268496B CN106268496B CN201610578298.3A CN201610578298A CN106268496B CN 106268496 B CN106268496 B CN 106268496B CN 201610578298 A CN201610578298 A CN 201610578298A CN 106268496 B CN106268496 B CN 106268496B
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- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K23/00—Use of substances as emulsifying, wetting, dispersing, or foam-producing agents
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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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- 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 using it as the clean fracturing fluid of thickening agent, prepare that simple, at low cost, the microcosmic reticular structure of clean fracturing fluid materials is apparent, viscoplasticity is good, superior, the broken glue of outstanding grittiness is thorough using this method, its biggest advantage is that temperature tolerance is good, best product is not less than 130mPas in 160 DEG C of shear viscosities below, the 25mPas required much larger than clean fracturing fluid site operation.
Description
Technical field
The present invention relates to oil-gas field development technical field, more particularly, to a kind of Shuangzi amphoteric viscoelastic surfactant and
Preparation method and using it as the clean fracturing fluid of thickening agent.
Background technology
The world today, the epoch for making oil go out from underground gurgle by stratum natural energy have terminated, and the whole world is most
Large-scale Thief zone oil gas field comes into the exploitation later stage, and demand of the countries in the world to oil is but in lasting rising, domestic and international oil
The troop of exploration and exploitation starts to march to hypotonic, Oil in Super-low Permeability and unconventional marginal oil-gas reservoir, and reservoir fracturing improvement, which becomes, to be carried
The key of high oil recovery factor, requirement of the oil field production to reservoir development degree and fracturing reform efficiency is continuously improved, conventional
Reservoir reconstruction (including reforming technology and working solution) exposes various drawbacks, especially with unconventional shale gas, fine and close oil
Deng exploitation, conventional reservoir reconstruction has been unable to meet the requirement of current fracturing reform, and " spirit of the working solution as reservoir reconstruction
Soul ", its quality decide that the success or failure of modification measures, the research and development of high performance operation liquid change as current untraditional reservoir reservoir
Make middle urgent problem to be solved.
Successful application of the Schlumberger in 1997 by viscoelastic surfactant fracturing fluid in reservoir fracturing improvement, starts
The research boom of clean fracturing fluid, to the low-grade oil and gas reservoir High Efficiency Reform in the world provides possibility.This fracturing fluid with often
Advise polymer fracturing fluid it is maximum difference lies in, it belongs to structural fluid, is shown as typical elastic fluid in a shear condition,
There is good prop-carrying capacity under low viscosity, broken natural or man-made polymer's fracturing fluid and relied on fluid viscosity suspended prop
Normal mode, to be conducive to the formation in long crack at a low viscosity, and breaking glue solution without residue, there is cleaning crack wall surface
Effect, fracture condudtiviy is can effectively improve, to receive the extensive concern of oilfield.
But due to the side such as unstability of surfactant under the conditions ofs high temperature, with high salt etc. and its dosage, cost
The reason of face, application of the clean fracturing fluid in reservoir reconstruction receive serious limitation.It dashes forward existing for current clean fracturing fluid
Ging wrong has:(1) use cost is high, and the viscoelastic surfactant that such as clean fracturing fluid of current document report uses is to pass
The single tail surface active agent of system, critical micelle concentration is higher, and dosage is too big in practical application, of high cost;(2) according to the literature,
Applicable formation temperature is generally less than 120 DEG C, and existing clean fracturing fluid technology can not be applied on the stratum of higher temperature;(3) strong
Stability is poor in electrolyte, and the ability of the especially metal ion of resistance to divalent is lower, and saponification or salt are easy to happen in concentrated water
Phenomenon is analysed, causes clean fracturing fluid that can not use.
Invention content
The present invention proposes a kind of Shuangzi amphoteric viscoelastic surfactant and preparation method thereof and using it as the clear of thickening agent
Clean fracturing fluid can solve the problems, such as that temperature tolerance is poor, of high cost, preparation process is complicated existing for existing clean fracturing liquid system.
What a kind of technical solution of the present invention was realized in:A kind of Shuangzi amphoteric viscoelastic surfactant, has
Following general structure:
Wherein R is the aliphatic unsaturated hydrocarbon of carbon atom number 18-21.
What the another technical solution of the present invention was realized in:A kind of preparation of Shuangzi amphoteric viscoelastic surfactant
Method includes the following steps:
(1) the 2 of 10mmol, 2 bis- (bromomethyl) -1,3-PDs are added in round-bottomed flask, are molten with tetrahydrofuran
The fatty acid amide propyl dimethylamine of 20mmol is added in agent, and 60 DEG C are flowed back 12 hours, wherein n (2,2 bis- (bromomethyl) -1,3- third
Glycol):N (fatty acid amide propyl dimethylamine)=1:2, vacuum distillation after reaction obtains intermediate A;
(2) intermediate A that the first step obtains is dissolved with tetrahydrofuran, the sodium hydride of 20~22mmol is added, room temperature stirs
Mix 15min, then will the 1,3-propane sultone of 20mmol with 50mL tetrahydrofurans dissolve after, be slowly dropped to intermediate A and
In the solution of sodium hydride reaction, 60 DEG C are flowed back 12 hours, wherein n (intermediate A):N (sodium hydride):N (1,3-propane sultone)
=1:2~2.2:2, it is reacted after reaction with extra sodium hydride with hydrochloric acid, is evaporated under reduced pressure after filtering and obtains clear yellow viscous glue
Shape Shuangzi amphoteric viscoelastic surfactant.
As a kind of perferred technical scheme, mole dosage of sodium hydride should be the 2~2.2 of intermediate A in reaction process
Times.
As a kind of perferred technical scheme, the aliphatic acid is stearic acid, oleic acid, arachidic acid or erucic acid.
What the another technical solution of the present invention was realized in:A kind of application Shuangzi amphoteric viscoelastic surfactant is
The clean fracturing fluid of thickening agent includes according to mass fraction:1.8~4.3% viscoelastic surfactant, 0.8~1.1%
Counter ion salt or inorganic salts, the water composition of surplus.
As a kind of perferred technical scheme, the counter ion or inorganic salts include potassium chloride, ammonium chloride, sodium salicylate,
Sodium benzoate, benzoic acid hydrogen potassium, carboxyl benzene sulfonate and the one such or several mixing of sulfosalicylic acid sodium salt.
As a kind of perferred technical scheme, the preparation of the clean fracturing fluid only needs mass fraction to be 1.4~4.3%
Viscoelastic surfactant be added to dissolved with mass fraction be 0.8~1.1% counter ion salt aqueous solution in, stirring to completely it is molten
Solution.
The present invention provides a kind of method preparing Shuangzi amphoteric salt viscoelastic surfactant using aliphatic acid, Yi Jili
The method for preparing clean fracturing fluid with the viscoelastic surfactant, prepared clean fracturing fluid can be protected at 160 DEG C or less
Excellent viscoplasticity is held, the fracturing fluid storey increase design of middle low permeability reservoir is can be used for.
Above-mentioned technical proposal is used, beneficial effects of the present invention are:
(1) preparation method of thickening agent is simple, and product yield is high, generally reaches 98% or more, impurity is few, to properties of product
Influence it is smaller.
(2) dosage is few, at low cost, uses the critical micelle concentration of the viscoelastic surfactant of above method preparation for 2
~3 × 10-4Mol/L, 1~2 order of magnitude lower than conventional 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 is logical
It crosses addition auxiliary agent and can be only achieved 135 DEG C, cause the composition of system more complicated, cost increases, best cleaning provided by the invention
Fracturing fluid is in 159 DEG C, 170s-1Condition down cut 1 hour, viscosity is maintained at 130mPas or more, has excellent viscoplasticity.
(4) clean fracturing fluid is prepared simple, it is only necessary to which the thickening agent of required quality is added to certain density counter ion salt
In aqueous solution, stirring to dissolving.
Description of the drawings
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technology description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
Some embodiments of invention without having to pay creative labor, may be used also for those of ordinary skill in the art
With obtain other attached drawings according to these attached drawings.
Fig. 1 is in embodiment one with the rheological curve of the 4.3% thickening agent+1.1%KCl clean fracturing fluids prepared
Fig. 2 is in embodiment one with the rheological curve of the 1.8% thickening agent+0.8%KCl clean fracturing fluids prepared
Fig. 3 is in embodiment two with the rheological curve of the 4.3% thickening agent+1.1%KCl clean fracturing fluids prepared
Fig. 4 is in embodiment two with the rheological curve of the 1.8% thickening agent+0.8%KCl clean fracturing fluids prepared
Fig. 5 is in embodiment three with the rheological curve of the 4.3% thickening agent+1.1%KCl clean fracturing fluids prepared
Fig. 6 is in embodiment three with the rheological curve of the 1.8% thickening agent+0.8%KCl clean fracturing fluids prepared
Fig. 7 is in example IV with the rheological curve of the 4.3% thickening agent+1.1%KCl clean fracturing fluids prepared
Fig. 8 is in example IV with the rheological curve of the 1.8% thickening agent+0.8%KCl clean fracturing fluids prepared
Specific implementation mode
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation describes, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, those of ordinary skill in the art are obtained every other without creative efforts
Embodiment shall fall within the protection scope of the present invention.
A kind of Shuangzi amphoteric viscoelastic surfactant, has following structure general formula:
Wherein R is the aliphatic unsaturated hydrocarbon of carbon atom number 18-21.
Embodiment one:
The 2 of 10mmol, 2 bis- (bromomethyl) -1,3-PDs are added in round-bottomed flask, using tetrahydrofuran as solvent,
The erucyl amide diemethylamine of 20mmol is added, 60 DEG C are flowed back 12 hours, wherein n (2,2 bis- (bromomethyl) -1,3- the third two
Alcohol):N (erucyl amide diemethylamine)=1:2, vacuum distillation after reaction obtains intermediate A.During the first step is obtained
Mesosome A is dissolved with tetrahydrofuran, and the sodium hydride of 20~22mmol, stirring at normal temperature 15min, then by the 1 of 20mmol, 3 third is added
After the tetrahydrofuran dissolving of 50mL of alkane sultone, it is slowly dropped in the solution of intermediate A and sodium hydride reaction, 60 DEG C of reflux
12 hours, wherein n (intermediate A):N (sodium hydride):N (1,3 propane sultone)=1:2~2.2:2, hydrochloric acid is used after reaction
It is reacted with extra sodium hydride, is evaporated under reduced pressure after filtering and obtains clear yellow viscous glue Shuangzi amphoteric viscoelastic surfactant.
The critical micelle concentration of the surfactant arrived is 3.63 × 10-4Mol/L, 4.3% thickening agent+1.1%KCl and 1.8% thickening
The clean fracturing fluid that agent+0.8%KCl is prepared is respectively in 159 DEG C, 170s-1With 119 DEG C, 170s-1Rheological characteristic such as attached drawing 1 and attached
Shown in Fig. 2, without apparent sedimentation, with 30% kerosene, breaking glue solution viscosity is 0 to the outstanding sand of static state after breaking gel within 2 hours.
Embodiment two:
The 2 of 10mmol, 2 bis- (bromomethyl) -1,3-PDs are added in round-bottomed flask, using tetrahydrofuran as solvent,
The arachidamide diemethylamine of 20mmol is added, 60 DEG C are flowed back 12 hours, wherein n (2,2 bis- (bromomethyl) -1,3- the third two
Alcohol):N (arachidamide diemethylamine)=1:2, vacuum distillation after reaction obtains intermediate A.The first step is obtained
Intermediate A is dissolved with tetrahydrofuran, and the sodium hydride of 20~22mmol, stirring at normal temperature 15min, then by the 1,3 of 20mmol is added
After the propane sultone tetrahydrofuran dissolving of 50mL, it is slowly dropped in the solution of intermediate A and sodium hydride reaction, 60 DEG C are returned
Stream 12 hours, wherein n (intermediate A):N (sodium hydride):N (1,3 propane sultone)=1:2~2.2:2, salt is used after reaction
It is sour to be reacted with extra sodium hydride, it is evaporated under reduced pressure after filtering and obtains clear yellow viscous glue Shuangzi amphoteric viscoelastic surfactant.
The critical micelle concentration of obtained surfactant is 3.63 × 10-4Mol/L ,+1.1% sodium salicylate of 4.3% thickening agent and
The clean fracturing fluid that+0.8% sodium salicylate of 1.8% thickening agent is prepared is respectively in 159 DEG C, 170s-1With 119 DEG C, 170s-1Stream
As shown in attached drawing 3 and attached drawing 4, the apparent sedimentation of 2 hours nothings of the outstanding sand of static state is with the breaking glue solution viscosity of 30% kerosene after breaking gel for denaturation
0。
Embodiment three:
The 2 of 10mmol, 2 bis- (bromomethyl) -1,3-PDs are added in round-bottomed flask, using tetrahydrofuran as solvent,
The oleamide diemethylamine of 20mmol is added, 60 DEG C are flowed back 12 hours, wherein n (2,2 bis- (bromomethyl) -1,3- the third two
Alcohol):N (oleamide diemethylamine)=1:2, vacuum distillation after reaction obtains intermediate A.During the first step is obtained
Mesosome A is dissolved with tetrahydrofuran, and the sodium hydride of 20~22mmol, stirring at normal temperature 15min, then by the 1 of 20mmol, 3 third is added
After the tetrahydrofuran dissolving of 50mL of alkane sultone, it is slowly dropped in the solution of intermediate A and sodium hydride reaction, 60 DEG C of reflux
12 hours, wherein n (intermediate A):N (sodium hydride):N (1,3 propane sultone)=1:2~2.2:2, hydrochloric acid is used after reaction
It is reacted with extra sodium hydride, is evaporated under reduced pressure after filtering and obtains clear yellow viscous glue Shuangzi amphoteric viscoelastic surfactant.
The critical micelle concentration of the surfactant arrived is 3.63 × 10-4Mol/L, 4.3% thickening agent+0.8%KCl and 1.8% thickening
The clean fracturing fluid that+1.1% sodium salicylate of agent is prepared is respectively in 159 DEG C, 170s-1With 119 DEG C, 170s-1Rheological characteristic such as attached drawing
5 and attached drawing 6 shown in, without apparent sedimentation, with 30% kerosene, breaking glue solution viscosity is 0 to the outstanding sand of static state after breaking gel within 2 hours.
Example IV:
The 2 of 10mmol, 2 bis- (bromomethyl) -1,3-PDs are added in round-bottomed flask, using tetrahydrofuran as solvent,
The stearic amide diemethylamine of 20mmol is added, 60 DEG C are flowed back 12 hours, wherein n (2,2 bis- (bromomethyl) -1,3- the third two
Alcohol):N (stearic amide diemethylamine)=1:2, vacuum distillation after reaction obtains intermediate A.The first step is obtained
Intermediate A is dissolved with tetrahydrofuran, and the sodium hydride of 20~22mmol, stirring at normal temperature 15min, then by the 1,3 of 20mmol is added
After the propane sultone tetrahydrofuran dissolving of 50mL, it is slowly dropped in the solution of intermediate A and sodium hydride reaction, 60 DEG C are returned
Stream 12 hours, wherein n (intermediate A):N (sodium hydride):N (1,3 propane sultone)=1:2~2.2:2, salt is used after reaction
It is sour to be reacted with extra sodium hydride, it is evaporated under reduced pressure after filtering and obtains clear yellow viscous glue Shuangzi amphoteric viscoelastic surfactant.
The critical micelle concentration of obtained surfactant is 3.63 × 10-4Mol/L ,+1.0% sodium salicylate of 4.0% thickening agent and
The clean fracturing fluid that 2.2% thickening agent+0.8%KCl is prepared is respectively in 159 DEG C, 170s-1With 119 DEG C, 170s-1Rheological characteristic such as
Shown in attached drawing 7 and attached drawing 8, the outstanding sand of static state settles for 2 hours without apparent, is 0 with the breaking glue solution viscosity of 30% kerosene after breaking gel.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
With within principle, any modification, equivalent replacement, improvement and so on should all be included in the protection scope of the present invention god.
Claims (5)
1. a kind of Shuangzi amphoteric viscoelastic surfactant, which is characterized in that it has following structure general formula:
Wherein R is the aliphatic unsaturated hydrocarbon of carbon atom number 18-21.
2. a kind of preparation method of Shuangzi amphoteric viscoelastic surfactant, which is characterized in that include the following steps:
(1)By the 2 of 10mmol, 2 pairs(Bromomethyl)1,3-PD is added in round-bottomed flask, using tetrahydrofuran as solvent, is added
Enter the fatty acid amide propyl dimethylamine of 20mmol, 60 DEG C are flowed back 12 hours, wherein n(2,2 pairs(Bromomethyl)- 1,3- the third two
Alcohol):n(Fatty acid amide propyl dimethylamine)= 1:2, vacuum distillation after reaction obtains intermediate A, the fatty acid amide
Diemethylamine is erucyl amide diemethylamine, arachidamide diemethylamine, oleamide diemethylamine or tristearin
Any one of sour amido propyl dimethylamine;
(2)The intermediate A that the first step obtains is dissolved with tetrahydrofuran, the sodium hydride of 20 ~ 22mmol, stirring at normal temperature is added
15min is slowly dropped to intermediate A and hydrogen after then dissolving the 1,3-propane sultone of 20mmol with 50mL tetrahydrofurans
In the solution for changing sodium reaction, 60 DEG C are flowed back 12 hours, wherein n(Intermediate A):n(Sodium hydride):n(1,3-propane sultone)=
1:2~2.2:2, it is reacted after reaction with extra sodium hydride with hydrochloric acid, is evaporated under reduced pressure after filtering and obtains gluey pair of clear yellow viscous
Sub- amphoteric viscoelastic surfactant.
3. a kind of preparation method of Shuangzi amphoteric viscoelastic surfactant as claimed in claim 2, which is characterized in that reaction
Mole dosage of sodium hydride is 2 ~ 2.2 times of intermediate A in the process.
4. it is a kind of using the clean fracturing fluid that Shuangzi amphoteric viscoelastic surfactant described in claim 1 is thickening agent, it is special
Sign is, includes according to mass fraction:1.8 ~ 4.3% viscoelastic surfactant, 0.8 ~ 1.1% counter ion salt or inorganic
Salt, the water composition of surplus.
5. clean fracturing fluid as claimed in claim 4, which is characterized in that the counter ion salt or inorganic salts include potassium chloride,
One or more of ammonium chloride, sodium salicylate, sodium benzoate, benzoic acid hydrogen potassium, carboxyl benzene sulfonate and sulfosalicylic acid sodium salt
Mixing.
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CN103074049B (en) * | 2013-01-21 | 2015-04-08 | 西南石油大学 | Fracturing fluid prepared by recovery waste water of crude oil and preparation method of fracturing fluid |
CN103301780A (en) * | 2013-06-28 | 2013-09-18 | 西南石油大学 | Twin-head viscoelastic surfactant and synthetic method thereof |
CN105080424A (en) * | 2015-09-02 | 2015-11-25 | 西南石油大学 | Cationic viscoelastic surfactant and preparation and application thereof |
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