CN106317320A - Hydrophobically associated polymer thickening agent and preparation method thereof - Google Patents
Hydrophobically associated polymer thickening agent and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a hydrophobically associated polymer thickening agent. The polymer thickening agent is a copolymer of five monomers of acrylate, a hydrophobically associated monomer, p-styrene sulfonate, 2-acrylamide-2-methyl propane sulfonic acid, and acrylamide. The polymer thickening agent has the advantages of short swelling time, good temperature-resistant, salt-resistant and shearing-resistant performances, rapid gel breaking, low damage to a reservoir, good resistance reducing effect, low cost, etc.
Description
Technical field
The invention belongs to oil gas field stimulation technology field, be specifically related to a kind of hydrophobic associated polymer thickening agent
And preparation method thereof.
Background technology
The fracturing fluid thickener that oil field uses at present mainly includes natural plant and derivatives class, viscoelasticity table
Face activating agent (VES) class and synthesized polymer species.It is the most biological to there is fracturing fluid in natural plant and derivant thereof
Degraded, high, the broken glue of water insoluble matter content are not thoroughly and the shortcoming such as injury is big；The injury of VES fracturing fluid fracture
Low, after breaking gel without residue, but heat resistance poor (being usually no more than 110 DEG C) and cost are high；Polyacrylamide
The traditional polymer fracturing fluid shortcoming such as amine, polyacrylate be heat-resistant salt-resistant resistant to shearing poor performance, broken glue not thoroughly,
Big to reservoir damage, frictional resistance is big.
Therefore, the problem that presently, there are is to need that a kind of swelling time of research and development is short, heat-resistant salt-resistant endurance of cutting
Energy is good, broken, and glue is rapid, little to reservoir damage, resistance reducing effect good and the hydrophobic associated polymer thickening agent of low cost.
Summary of the invention
The technical problem to be solved is for the deficiencies in the prior art, it is provided that a kind of hydrophobic association polymerization
Thing thickening agent.This polymer viscosifier swelling time is short, heat-resistant salt-resistant resistant to shearing performance is good, hang grittiness energy and broken
Glue function admirable, and little to reservoir damage, can be used in high temperature with the fracturing fluid that this polymer viscosifier is prepared low
Ooze the pressing crack construction of reservoir.
To this end, first aspect present invention provides a kind of hydrophobic associated polymer thickening agent, its be acrylates,
Hydrophobic association monomer, p styrene sulfonic acid salt, 2-acrylamide-2-methyl propane sulfonic and five kinds of monomers of acrylamide
Copolymer, molecular weight is 500～10,000,000.
According to the present invention, described hydrophobic association monomer include alkyl acrylate, alkyl dimethyl ethyl ammonium bromide,
In 2-acrylamido-2-alkyl ethyl sulfonic acid or (2-methylacryloyl) oxygen ethyl dimethyl alkyl bromination ammonium
At least one, wherein the carbon number of alkyl is 8～18, and the preferably carbon number of alkyl is 12～16.
According to the present invention, in described polymer viscosifier, the ratio of five kinds of monomers is: acrylates and propylene
The mol ratio of amide is (0.01～0.40): 1；Hydrophobic association monomer is (9 × 10 with the mol ratio of acrylamide-4~
6×10-2):1；P styrene sulfonic acid salt is (6 × 10 with the mol ratio of acrylamide-5～2 × 10-3):1；2-propylene
Amide-2-methyl propane sulfonic acid is 5 × 10 with the mol ratio of acrylamide-4～2 × 10-2:1。
In some currently preferred embodiments of the present invention, in described polymer viscosifier, the ratio of five kinds of monomers is:
Acrylates is (0.03～0.38) with the mol ratio of acrylamide: 1；Hydrophobic association monomer rubs with acrylamide
Your ratio is (9.39 × 10-4～6 × 10-2):1；P styrene sulfonic acid salt with the mol ratio of acrylamide is
(6.89×10-5～1.72 × 10-3):1；2-acrylamide-2-methyl propane sulfonic with the mol ratio of acrylamide is
(6.86×10-4～1.72 × 10-2):1。
In some embodiments of the invention, during described acrylates includes acrylic acid sodium salt, potassium salt and lithium salts
At least one.The most described acrylates is sodium acrylate.
In some embodiments of the invention, described p styrene sulfonic acid salt include p styrene sulfonic acid sodium salt,
At least one in potassium salt and lithium salts.The most described p styrene sulfonic acid salt is sodium p styrene sulfonate.
Second aspect present invention provides the preparation of a kind of polymer viscosifier as described in the first aspect of the invention
Method, comprising:
Step A, prepares copolymerized monomer mixture: by acrylates, hydrophobic association monomer, p styrene sulfonic acid
Salt, 2-acrylamide-2-methyl propane sulfonic, acrylamide, urea and disodiumedetate are soluble in water, mixed
Copolymerized monomer mixture is prepared after closing uniformly；
Step B, polyreaction: copolymerized monomer mixture is existed at initiator and under oxygen free condition, carries out close
Close polyreaction, prepare gel polymer thickening agent.
In the present invention, described copolymerized monomer mixture composition by weight is as follows:
In above-mentioned copolymerized monomer mixture, urea and disodiumedetate are the reaction promoter of polyreaction.
According to the present invention, in stepb, described initiator includes redox initiator and azo-initiator.
According to the present invention, described redox initiator is made up of Oxidizing and Reducing Agents.
In the present invention, preferably in described redox initiator, oxidant is 1:1 with the mass ratio of reducing agent.
In some embodiments of the invention, during described oxidant is Ammonium persulfate., sodium peroxydisulfate and potassium peroxydisulfate
At least one.The most described oxidant is Ammonium persulfate..
In other embodiments of the present invention, described reducing agent is sodium sulfite, sodium sulfite and lays particular stress on Asia
At least one in sodium sulfate.The most described reducing agent is sodium sulfite.
According to the present invention, the addition of described redox initiator is in terms of copolymerized monomer mixture gross mass
0.01%～0.5%.The addition of described azo-initiator in terms of copolymerized monomer mixture gross mass 0.01%～
0.5%.
In the present invention, preferential oxidation reduction initiator is 1:1 with the mass ratio of azo-initiator
In some embodiments of the invention, described azo-initiator is azodiisobutyronitrile, azo two different heptan
Nitrile, at least one in azo two isobutyl imidazoline hydrochloride and azo-bis-isobutyrate hydrochloride.The most described idol
Nitrogen class initiator is azo-bis-isobutyrate hydrochloride.
According to the present invention, in stepb, described oxygen free condition is by being passed through inertia in airtight reactor
Gas realizes.It is to say, it is by close that copolymerized monomer mixture carries out polyreaction under anaerobic
The reactor closed is passed through what noble gas realized.Described noble gas includes but not limited to nitrogen and helium.
According to the present invention, in stepb, the temperature of described polyreaction is 50～90 DEG C.
According to the present invention, in stepb, the time of described polyreaction is 3～5 hours.
In certain embodiments of the present invention, step C is the most also included, by gel polymer
Thickening agent pelletize, be dried, pulverize and sieve after obtain white powder product, obtain dry polymer-thickened
Agent granule.
In the present invention, the particle diameter of the most described polymer viscosifier granule is 50～200 μm.
In the present invention, institute's term " water " word, in the case of not specifying, refers to deionized water.
In the present invention institute's term " copolymerized monomer mixture " refer to containing comonomer, reaction promoter (include urea and
Disodiumedetate) and the mixed reactant of water.
The liquid formed after institute's term " breaking glue solution " refers to fracturing liquid rubber-breaking in the present invention.
Polymer viscosifier provided by the present invention has the advantage that
(1) swelling time is short.Containing a large amount of hydrophilic functional groups in this polymer viscosifier, swelling time≤2
Minute, it is achieved dosing continuously, on-the-spot application is convenient.
(2) heat-resistant salt-resistant resistant to shearing performance is good.This polymer viscosifier is configured to fracturing fluid, and heat resistance reaches
160 DEG C, have anti-1 × 104Ppm salinity ability, fracturing fluid is pumped up, borehole and flow event will not be obvious
Destroying the rheological characteristic of liquid, anti-shear performance is good.
(3) broken glue is rapid.This polymer viscosifier is configured to fracturing fluid, breaking glue solution viscosity ＜ 2 in 2 hours
MPa s, does not the most produce insoluble matter, it is easy to accomplish the row of returning completely.
(4) low to reservoir damage.This polymer viscosifier is configured to fracturing fluid to rock core matrix damage rate ＜ 10%.
(5) resistance reducing effect is good.This polymer viscosifier resistance-reducing yield ＞ 60%, advantageously reduces ground pump pressure.
(6) without adding cleanup additive.This polymer viscosifier is configured to fracturing fluid, after breaking gel surface tension ＜
≤ 28mN/m, it is not necessary to separately with cleanup additive, saves construction cost.
(7) physical crosslinking.This polymer viscosifier contains a large amount of hydrophobic functional group, can with without metallic element
Low molecular compound produce physical crosslinking effect.
As can be seen here, polymer viscosifier provided by the present invention has that swelling time is short, heat-resistant salt-resistant resistant to shearing
Performance is good, broken, and glue is rapid, low to reservoir damage, resistance reducing effect good and low cost and other advantages.
Accompanying drawing explanation
Below in conjunction with accompanying drawing, the present invention is described.
Fig. 1 is fracturing fluid that in the embodiment of the present invention 1, polymer viscosifier the is configured to stream at a temperature of 160 DEG C
Varied curve.
Fig. 2 is fracturing fluid that in the embodiment of the present invention 2, polymer viscosifier the is configured to stream at a temperature of 160 DEG C
Varied curve.
Fig. 3 is fracturing fluid that in the embodiment of the present invention 3, polymer viscosifier the is configured to stream at a temperature of 160 DEG C
Varied curve.
Fig. 4 is fracturing fluid that in the embodiment of the present invention 4, polymer viscosifier the is configured to stream at a temperature of 160 DEG C
Varied curve.
Detailed description of the invention
For making the present invention easier to understand, describe the present invention in detail below in conjunction with embodiment and accompanying drawing, this
A little embodiments only play illustrative effect, it is not limited to the range of application of the present invention.
Raw materials used in embodiment it is analytical pure.Embodiment relates in the reference of fracturing fluid property assay method
China people's republic's oil and gas industry standard " SY/T5107-2005 aqueous fracturing fluid method of evaluating performance " and
" SY/T6376-2008 fracturing fluid general technical specifications ".
In the present invention, the particle diameter of polymer viscosifier uses ANALYSETTE22MicroTec plus type laser
Particle size instrument (moral good fortune Ritz instrument and equipment company limited).
In the present invention, the molecular weight of thickening agent uses viscosity method to measure: be dissolved in by testing sample identical molten
Being made into the solution of a series of variable concentrations in agent, (Shanghai is close logical to use SBQ81834 type Ubbelohde viscosimetric analysis device
Electromechanical Technology Co., Ltd) its viscosity of mensuration under the conditions of 25 ± 0.05 DEG C, and thus calculate this and treat test sample
The intrinsic viscosity of product, then calculates molecular weight further according to Mark-Houwink equation [η]=KM α.
The formula of fracturing fluid described in embodiment is: the thickening agent of 0.6% (weight), the friendship of 0.3% (weight)
Connection agent, the clay stabilizer of 0.3% (weight) and the gel breaker of 0.001% (weight).
Embodiment
Embodiment 1: prepare polymer viscosifier.
(1) be separately added in 300g deionized water 15g sodium acrylate, 2.3g acrylic acid hexadecanol ester,
100g acrylamide, 0.1g sodium p styrene sulfonate, 0.45g 2-acrylamide-2-methylpro panesulfonic acid, 0.16
G urea and 0.2g disodiumedetate, be sufficiently stirred for dissolving, prepare copolymerized monomer mixture.
(2) in above-mentioned hybrid reaction system, 0.4g Ammonium persulfate., 0.4g sodium sulfite and 0.46g are added
Azo-bis-isobutyrate hydrochloride causes, reaction temperature 80 DEG C, and response time 3h obtains gel-like product,
Through pelletize, it is dried, pulverizes and sieves, obtain dry polymer viscosifier finished granule.
Through measuring, the molecular weight of this polymer viscosifier is 5,000,000, and the particle diameter of granule is 50～100 μm.
The fracturing fluid being configured to by this polymer viscosifier rheological curve at a temperature of 160 DEG C is shown in Fig. 1.
After testing, the swelling time of this polymer viscosifier is 2 minutes；The polymer viscosifier aqueous solution of 0.6%
Viscosity be 63mPa s；The resistance-reducing yield of the polymer viscosifier aqueous solution of 0.1% is 60.15%；By this polymer
The fracturing fluid that thickening agent is configured to is at 160 DEG C, 170S-1Under the conditions of shear 2h, average tail glues for 56.1mPa s,
Breaking glue solution viscosity is 1.84mPa s, and breaking glue solution surface tension is 25.7mN/m.
Embodiment 2: prepare polymer viscosifier.
(1) in 300g deionized water, it is separately added into 20g sodium acrylate, 3.1g hexadecyldimethyl benzyl ammonium second
Base ammonium bromide, 125g acrylamide, 0.2g sodium p styrene sulfonate, 0.68g 2-acrylamido-2-methyl
Propane sulfonic acid, 0.21g urea and 0.36g disodiumedetate, be sufficiently stirred for dissolving, and prepares comonomer and mixes
Compound.
(2) in above-mentioned hybrid reaction system, 0.5g Ammonium persulfate., 0.5g sodium sulfite and 0.6g are added
Azo-bis-isobutyrate hydrochloride causes, reaction temperature 85 DEG C, response time 3.5h, obtains gel and produces
Thing, through pelletize, is dried, pulverizes and sieves, and obtains dry polymer viscosifier finished granule.
Through measuring, the molecular weight of this polymer viscosifier is 6,800,000, and the particle diameter of granule is 60～130 μm.
The fracturing fluid being configured to by this polymer viscosifier rheological curve at a temperature of 160 DEG C is shown in Fig. 2.
After testing, the swelling time of this polymer viscosifier is 2 minutes；The polymer viscosifier aqueous solution of 0.6%
Viscosity is 60mPa s；The resistance-reducing yield of the polymer viscosifier aqueous solution of 0.1% is 61.35%；Increased by this polymer
The thick dose of fracturing fluid being configured to is at 160 DEG C, 170S-1Under the conditions of shear 2h, average tail glues for 55.4mPa s,
Breaking glue solution viscosity is 1.95mPa s, and breaking glue solution surface tension is 25.2mN/m.
Embodiment 3: prepare polymer viscosifier.
(1) in 300g deionized water, it is separately added into 25g sodium acrylate, 4.2g 2-acrylamido-2-ten
Six alkyl ethyl sulfonic acids, 150g acrylamide, 0.3g sodium p styrene sulfonate, 0.75g 2-acrylamido-2-
Methyl propane sulfonic acid, 0.3g urea and 0.45g disodiumedetate, be sufficiently stirred for dissolve, prepare comonomer
Mixture.
(2) in above-mentioned hybrid reaction system, 0.6g Ammonium persulfate., 0.6g sodium sulfite and 0.78g are added
Azo-bis-isobutyrate hydrochloride causes, reaction temperature 90 DEG C, and response time 4h obtains gel-like product,
Through pelletize, it is dried, pulverizes and sieves, obtain dry polymer viscosifier finished granule.
Through measuring, the molecular weight of this polymer viscosifier is 8,500,000, and the particle diameter of granule is 120～180 μm.
The fracturing fluid being configured to by this polymer viscosifier rheological curve at a temperature of 160 DEG C is shown in Fig. 3.
After testing, the swelling time of this polymer viscosifier is 2 minutes；The polymer viscosifier aqueous solution of 0.6%
Viscosity is 66mPa s；The resistance-reducing yield of the polymer viscosifier aqueous solution of 0.1% is 60.52%；Increased by this polymer
The breaking glue solution of the thick dose of fracturing fluid being configured to is at 160 DEG C, 170S-1Under the conditions of shear 2h, it is 54.6 that average tail glues
MPa s, breaking glue solution viscosity is 1.12mPa s, and breaking glue solution surface tension is 24.7mN/m.
Embodiment 4: prepare polymer viscosifier.
(1) in 300g deionized water, it is separately added into 30g sodium acrylate, 5.6g (2-methylacryloyl)
Oxygen ethyl dimethyl hexadecyl base ammonium bromide, 200g acrylamide, 0.4g sodium p styrene sulfonate, 0.86g 2-
Acrylamide-2-methylpro panesulfonic acid, 0.4g urea and 0.58g disodiumedetate, be sufficiently stirred for dissolve,
Prepare copolymerized monomer mixture.
(2) in above-mentioned hybrid reaction system, 0.8g Ammonium persulfate., 0.8g sodium sulfite and 0.85g are added
Azo-bis-isobutyrate hydrochloride causes, reaction temperature 90 DEG C, and response time 5h obtains gel-like product,
Through pelletize, it is dried, pulverizes and sieves, obtain dry polymer viscosifier finished granule.
Through measuring, the molecular weight of this polymer viscosifier is 10,000,000, and the particle diameter of granule is 140～200 μm.
The fracturing fluid being configured to by this polymer viscosifier rheological curve at a temperature of 160 DEG C is shown in Fig. 4.
After testing, the swelling time of this polymer viscosifier is 2 minutes；The polymer viscosifier aqueous solution of 0.6%
Viscosity is 69mPa s；The resistance-reducing yield of the polymer viscosifier aqueous solution of 0.1% is 60.84%；Increased by this polymer
The thick dose of fracturing fluid being configured to is at 160 DEG C, 170S-1Under the conditions of shear 2h, average tail glues for 52.1mPa s, broken
Gelatin viscosity is 1.45mPa s, and breaking glue solution surface tension is 25.1mN/m.
The fracturing fluid being configured to above-mentioned polymer viscosifier carries out resistance to salinity and cut resistance test, result table
Bright, this polymer viscosifier is configured to fracturing fluid, has anti-1 × 104Ppm salinity ability, and fracturing fluid warp
Pumping, borehole and flow event will not substantially destroy the rheological characteristic of liquid, and anti-shear performance is good.
It addition, the fracturing fluid being configured to above-mentioned polymer viscosifier carries out the result table of rock core matrix damage test
Bright, this polymer viscosifier is configured to fracturing fluid to rock core matrix damage rate ＜ 10%.
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 in the protection of the present invention
Within the scope of.
Claims (10)
1. a hydrophobic associated polymer thickening agent, its be acrylates, hydrophobic association monomer, to styrene sulphur
Hydrochlorate, 2-acrylamide-2-methyl propane sulfonic and the copolymer of five kinds of monomers of acrylamide.
Polymer viscosifier the most according to claim 1, it is characterised in that described hydrophobic association monomer bag
Include alkyl acrylate, alkyl dimethyl ethyl ammonium bromide, 2-acrylamido-2-alkyl ethyl sulfonic acid and (2-first
Base acryloyl group) at least one in oxygen ethyl dimethyl alkyl bromination ammonium, wherein the carbon number of alkyl be 8～
18, the preferably carbon number of alkyl is 12～16.
Polymer viscosifier the most according to claim 1 and 2, it is characterised in that the ratio of five kinds of monomers
For: acrylates is (0.01～0.40) with the mol ratio of acrylamide: 1；Hydrophobic association monomer and acrylamide
Mol ratio be (9 × 10-4～6 × 10-2):1；P styrene sulfonic acid salt is (6 × 10 with the mol ratio of acrylamide-5~
2×10-3):1；2-acrylamide-2-methyl propane sulfonic is 5 × 10 with the mol ratio of acrylamide-4～2 × 10-2:1。
4. according to the polymer viscosifier described in any one in Claim 1-3, it is characterised in that described
Acrylates includes at least one in acrylic acid sodium salt, potassium salt and lithium salts；The most described acrylates is third
Olefin(e) acid sodium；Described p styrene sulfonic acid salt includes at least in the sodium salt of p styrene sulfonic acid, potassium salt and lithium salts
Kind；The most described p styrene sulfonic acid salt is sodium p styrene sulfonate.
5. a preparation method for polymer viscosifier as described in any one in claim 1 to 4, comprising:
Step A, prepares copolymerized monomer mixture: by acrylates, hydrophobic association monomer, p styrene sulfonic acid
Salt, 2-acrylamide-2-methyl propane sulfonic, acrylamide, urea and disodiumedetate are soluble in water, mixed
Copolymerized monomer mixture is prepared after closing uniformly；
Step B, polyreaction: copolymerized monomer mixture is existed at initiator and under oxygen free condition, carries out close
Close polyreaction, prepare gel polymer thickening agent.
Preparation method the most according to claim 5, it is characterised in that described copolymerized monomer mixture is by weight
The composition of gauge is as follows:
7. according to the preparation method described in claim 5 or 6, it is characterised in that in stepb, described in draw
Send out agent and include redox initiator and azo-initiator.
Preparation method the most according to claim 7, it is characterised in that adding of described redox initiator
Entering amount is 0.01% in terms of copolymerized monomer mixture gross mass～0.5%；The addition of described azo-initiator
In terms of copolymerized monomer mixture gross mass 0.01%～0.5%.
9. according to the preparation method described in any one in claim 5 to 8, it is characterised in that described polymerization
The temperature of reaction is 50～90 DEG C.
10. according to the preparation method described in any one in claim 5 to 9, it is characterised in that described poly-
The time closing reaction is 3～5 hours.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106867488A (en) * | 2017-03-28 | 2017-06-20 | 四川光亚聚合物化工有限公司 | One kind physical crosslinking gel-like profile control and water plugging system and its application |
| CN112322274A (en) * | 2020-11-27 | 2021-02-05 | 西安石油大学 | Preparation method of repeatable water-based fracturing fluid, gel breaker and application of gel breaker |
| CN113372488A (en) * | 2021-06-30 | 2021-09-10 | 华美孚泰油气增产技术服务有限责任公司 | Saline-based fracturing fluid thickening agent with reverse polyelectrolyte behavior and preparation method thereof |
| CN118047905A (en) * | 2024-04-16 | 2024-05-17 | 中海油天津化工研究设计院有限公司 | Five-membered hydrophobically associating modified acrylamide polymer, preparation method thereof, suspension type thickening agent and fracturing fluid |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106867488A (en) * | 2017-03-28 | 2017-06-20 | 四川光亚聚合物化工有限公司 | One kind physical crosslinking gel-like profile control and water plugging system and its application |
| CN112322274A (en) * | 2020-11-27 | 2021-02-05 | 西安石油大学 | Preparation method of repeatable water-based fracturing fluid, gel breaker and application of gel breaker |
| CN113372488A (en) * | 2021-06-30 | 2021-09-10 | 华美孚泰油气增产技术服务有限责任公司 | Saline-based fracturing fluid thickening agent with reverse polyelectrolyte behavior and preparation method thereof |
| CN118047905A (en) * | 2024-04-16 | 2024-05-17 | 中海油天津化工研究设计院有限公司 | Five-membered hydrophobically associating modified acrylamide polymer, preparation method thereof, suspension type thickening agent and fracturing fluid |
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Application publication date: 20170111 |