CN105601840B - A kind of acrylamide/sodium Acrylate multiple copolymer, preparation method and emulsion-type aqueous fracturing fluid drag reducer - Google Patents
A kind of acrylamide/sodium Acrylate multiple copolymer, preparation method and emulsion-type aqueous fracturing fluid drag reducer Download PDFInfo
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Abstract
The invention discloses a kind of acrylamide/sodium Acrylate multiple copolymer, preparation method and emulsion-type aqueous fracturing fluid drag reducer, which contains four kinds of structural units shown in Formulas I~formula IV；Preparation method includes：1) organic solvent is mixed into obtain oil phase with emulsifier；Reaction monomers are added to the water, aqueous solution is made, adjust pH with sodium hydroxide obtains water phase for 7.0~7.5；Reaction monomers are acrylamide, acrylic acid, 2 acrylamide, 2 methyl propane sulfonic acid and diallyl polyether；2) stirring in oil phase is added in water phase makes its emulsification, be added initiator polymerize to get.For the multiple copolymer as drag reducer in use, mass concentration is 0.06%~0.15%, apparent viscosity is 6~21mPa.s, and drag reducing efficiency >=65% has good resistance reducing performance；Initial apparent viscosity is big simultaneously, breaks glue speed and accelerates, has excellent broken colloidality energy.
Description
Technical field
The invention belongs to oil gas field drag reduction fracturing fluid technical fields, and in particular to a kind of acrylamide/sodium Acrylate is polynary
Copolymer and preparation method thereof also relates to a kind of emulsion-type water using the acrylamide/sodium Acrylate multiple copolymer
Base fracturing fluid drag reducer.
Background technology
With unconventional petroleum resources upsurge is exploited to start, hydraulic fracturing as frscturing technical measures oneself increasingly
Show importance, (a small amount of drag reduction is added in the drag reduction water fracturing technique suitable for exploiting hyposmosis unconventional reservoir clear water
Agent and some additives etc. are used as working solution, and when construction and the fracturing work of a small amount of proppant is added) increasingly promoted, because
This, the application of the use of additive, especially drag reducer and demand are also more and more in slippery water fracturing fluid.
Drag reducing agent product currently on the market is mostly cation, nonionic polyacrylamides solid powder or lotion.Sun
Ion or non-ionic polyacrylamide solid powder or lotion are intolerant to hard water；Due to the limitation of molecular structure, under high speed shear
Strand can degrade, and at the scene under pressure break working condition, cannot embody preferable resistance reducing performance；Meanwhile cation or
Non-ionic polymers are easily adsorbed by stratum, and flocculation is easy tod produce in the case of having impurity in water.Such polyacrylamide
Polymer is not degradable in the earth formation, can cause permanent injury to stratum.So such product is not suitable for live fracturing work.
In the prior art, some contain the hydrophilic radicals such as sulfonic group, carboxyl and the vinyl polymerization monomer of huge side group
It is used to carry out modification by copolymerization with acrylamide, to improve the performance of drag reducer.But existing drag reducer polymer line
Property structure main chain on, structural unit be mostly-C-C-, have stronger rigidity, be not easy to unfold in the solution, friction loss compared with
Greatly, drag-reduction effect is not met by the requirement used.As CN105037621A discloses a kind of modified brine drag reducer, the halogen
Water drag reducer is poly- (acrylamide -2- acrylamide-2-methylpro panesulfonic acids-itaconic acid), and structural formula is：
Wherein, m, n, p are the natural number of non-zero, and molecular weight is 3 × 106More than.Preparation method is by non-ionic monomer, resistance to
The resistance to salt monomer of temperature, cationic monomer carry out aqueous solution polymerization in redox initiation system, obtain modified brine drag reducer；It is described
Non-ionic monomer be acrylamide, the heat-resistant salt-resistant monomer be 2- acrylamide-2-methylpro panesulfonic acids, described the moon
Ion monomer is itaconic acid；Using potassium peroxydisulfate/sodium hydrogensulfite as redox initiator, preferred reaction condition is,
In 40-60 DEG C of thermotonus 3-6h；After the completion of polymerisation, reaction solution is stood 24-30 hours under air-proof condition, makes polymerization
Product stable molding, insoluble impurity and the layering of unreacted monomer are precipitated.The brine drag reducer have good anti-salt property and
Preferable heat resistance, synthesis are simple；But drag reducing efficiency maximum only reaches 36.8%, and it is unconventional to be not met by hyposmosis
The requirement that the drag reduction hydraulic pressure of reservoir is split.
Invention content
The object of the present invention is to provide a kind of acrylamide/sodium Acrylate multiple copolymers, have as drag reducer good
Resistance reducing performance.
Second object of the present invention is to provide a kind of preparation method of acrylamide/sodium Acrylate multiple copolymer.
Third object of the present invention is to provide a kind of lotions using above-mentioned acrylamide/sodium Acrylate multiple copolymer
Type aqueous fracturing fluid drag reducer.
In order to achieve the goal above, the technical solution adopted in the present invention is：
A kind of acrylamide/sodium Acrylate multiple copolymer, the multiple copolymer contain four kinds of knots shown in Formulas I~formula IV
Structure unit：
In formula IV, EO is-OCH2CH2(epoxy ethyl), PO are-OCH (CH3)CH2(glycidyl)；0≤x<55,0≤
Y≤10,0≤z≤16 are 0 when x, y, z difference.
Preferably, the acrylamide/sodium Acrylate multiple copolymer, contains following structural formula：
Wherein, m, n, o, p are the quantity (mole) of each structural unit, and m, n, o, p are the natural number of non-zero.
The acrylamide/sodium Acrylate multiple copolymer of the present invention, on the basis of the linear structure of drag reducer copolymer, to
Hydrophily soft segment (diallyl polyether) is introduced on main chain, and compared with existing drag reducer copolymer, there is as follows excellent
Point：
1. due to main chain introducing-CH2CH2O-, high molecular polymer under high shear, be easier in the solution be in
Extended position is easy to happen distortion rotation, thus it is possible to vary the size and Orientation of fluid force makes a part of radial load be changed into
Fair current to axial force, to reduce the consumption of idle work, macroscopically play the role of reduce friction loss；
2. due to main chain introducing-CH2CH2O-, under the action of peroxide, C-O keys are more easily broken off relative to C-C keys,
The broken colloidality energy for macroscopically increasing drag reducer, advantageously reduces formation damage；
3. due to main chain introducing-CH2CH2The hydrophily of O-, main chain further enhance, and are conducive to the multiple copolymer conduct
Drag reducer swelling dissolving rapidly in various aquatic environments.
The efficient drag reduction of multiple copolymer low concentration, high concentration are cross-linking at frozen glue；It uses, has excellent as drag reducer
Resistance reducing performance and broken colloidality energy.
A kind of preparation method of above-mentioned acrylamide/sodium Acrylate multiple copolymer, includes the following steps：
1) organic solvent is mixed with emulsifier, obtains oil phase；Reaction monomers are added to the water, aqueous solution is made, uses hydroxide
It is 7.0~7.5 that sodium, which adjusts pH, obtains water phase；The reaction monomers are acrylamide, acrylic acid, 2- acrylamide -2- methyl-prop sulphurs
Acid and diallyl polyether；Wherein, shown in the following Formula IV of the structural formula of the diallyl polyether：
In Formula IV, EO is-OCH2CH2(epoxy ethyl), PO are-OCH (CH3)CH2(glycidyl)；0≤x<55,0≤
Y≤10,0≤z≤16 are 0 when x, y, z difference；
2) water phase obtained by step 1) is added in oil phase obtained by step 2), after stirring makes it emulsify, initiator is added and carries out
Polymerization to get.
In step 1), the organic solvent is any one or combination in hexamethylene, kerosene, white oil.
In step 1), the emulsifier is sorbitan monostearate (Span60), sorbitan monooleate
(Span80), in polyoxyethylene shrink sorbitol monooleate (Tween80), hypermer 1083, hypermer 1031
Any one is combined.Wherein, hypermer 1083, hypermer 1031 are big (the CRODA Geo of Britain's standing grain
Technologies) the polymerization ester type emulsifier provided.
In the step 1) reaction monomers, acrylamide, acrylic acid, 2- acrylamide-2-methyl propane sulfonics and diene third
The mass ratio of base polyethers is 100:8~30:5~30:1~15.The reaction monomers are water-soluble reaction monomer.Preferably,
In the step 1) reaction monomers, acrylamide, acrylic acid, 2- acrylamide-2-methyl propane sulfonics and diallyl polyether
Mass ratio is 100:8~15:8~15:10~15.
In step 1), after the pH with sodium hydroxide regulation system, nitrogen is passed through into system；The time of logical nitrogen is
20min.The purpose of logical nitrogen is the oxygen in removing system.In above-mentioned preparation method, when preparing oil phase, water phase, temperature is controlled
≤30℃。
In step 2), when oil phase is added in water phase, the mass ratio of reaction monomers and organic solvent is 30~35:25~35.
The additive amount of emulsifier is the 2%~5% of reaction monomers gross mass.In the water phase, the mass ratio of reaction monomers and water is 30
~35:29~45.
In step 2), the rotating speed of stirring is 1500rpm；The time of stirring is 30min.During stirring, to system
It is inside passed through nitrogen, to ensure oxygen-free environment；Control temperature≤20 DEG C of stirring.
In step 2), the initiator is the oxidation that ammonium persulfate or potassium peroxydisulfate are formed with sodium hydrogensulfite or sodium formaldehyde sulfoxylate
Reduction initiating system.The additive amount of initiator is the 0.002%~0.5% of reaction monomers gross mass.Preferably, initiator adds
Dosage is the 0.015%~0.02% of reaction monomers gross mass.
Above-mentioned preparation method carries out in closed reactor.The closed reactor is equipped with insulation jacket.
In step 2) when polymerization, temperature≤80 DEG C of control system.In order to obtain the lotion of stable uniform particle sizes, pass through
Chuck controls temperature≤80 DEG C of reaction system.
The preparation method of the acrylamide/sodium Acrylate multiple copolymer of the present invention, with acrylamide, acrylic acid, 2- third
Acrylamide -2- methyl propane sulfonic acids are water-soluble reaction monomer with diallyl polyether, using the method for inverse emulsion polymerization, synthesis
Acrylamide/sodium Acrylate multiple copolymer realizes the introducing-CH on the main chain of copolymer linear structure2CH2The flexible base of O-
Group；The efficient drag reduction of multiple copolymer low concentration, high concentration are cross-linking at frozen glue；It is used as drag reducer, there is excellent subtract
Resistive energy and broken colloidality energy；The preparation method is simple for process, easy to operate, is suitble to large-scale industrial production.
A kind of emulsion-type aqueous fracturing fluid drag reducer contains above-mentioned acrylamide/sodium Acrylate multiple copolymer.
The emulsion-type aqueous fracturing fluid drag reducer also contains reverse phase surface activating agent, the reverse phase surface activating agent
For polyoxyethylene sorbitol acid anhydride trioleate (Tween85), fat alcohol polyethylene ether (AEO9), nonylphenol polyoxyethylene ether (OP-
10) any one in or combination.The addition quality of reverse phase surface activating agent is acrylamide/sodium Acrylate multiple copolymer
The 0.5%~6% of reaction monomers gross mass.
The acrylamide/sodium Acrylate multiple copolymer of the present invention is as drag reducer in use, mass concentration is 0.06%
~0.15%, apparent viscosity is 6~21mPa.s, and drag reducing efficiency >=65% has good resistance reducing performance；It is initial simultaneously apparent viscous
Degree is big, breaks glue speed and accelerates, has excellent broken colloidality energy.
The preparation method of above-mentioned acrylamide/sodium Acrylate multiple copolymer, includes the following steps：
1) organic solvent is mixed with emulsifier, obtains oil phase；Reaction monomers are added to the water, aqueous solution is made, uses hydroxide
It is 7.0~7.5 that sodium, which adjusts pH, obtains water phase；The reaction monomers are acrylamide, acrylic acid, 2- acrylamide -2- methyl-prop sulphurs
Acid and diallyl polyether；Wherein, shown in the following Formula IV of the structural formula of the diallyl polyether：
In Formula IV, EO is-OCH2CH2(epoxy ethyl), PO are-OCH (CH3)CH2(glycidyl)；0≤x<55,0≤
Y≤10,0≤z≤16 are 0 when x, y, z difference；
2) water phase obtained by step 1) is added in oil phase obtained by step 2), after stirring makes it emulsify, initiator is added and carries out
Polymerization, add reverse phase surface activating agent to get.
Further, reverse phase surface activating agent can be added simultaneously and adjust slippery water/gelled fracturing fluid as crosslinking agent
Apparent viscosity；What it is due to addition is reverse phase surface activity crosslinker agent, is returned in drain as the drag reducer and surface-active after degradation
Agent can be reused by simply detaching, or be reused after being mixed according to a certain percentage with clear water, be had good
Economic benefit and environmental benefit.
Description of the drawings
Fig. 1 is the drag reducing efficiency testing result schematic diagram of drag reducer obtained by embodiment 1-4 and comparative example.
Specific implementation mode
The present invention is further illustrated With reference to embodiment.
The acrylamide/sodium Acrylate multiple copolymer of embodiment, contains following structural formula：
Wherein, m, n, o, p are the quantity (mole) of each structural unit, and m, n, o, p are the natural number of non-zero.
The preparation method of the acrylamide/sodium Acrylate multiple copolymer of embodiment, includes the following steps：
1) in the closed reactor equipped with chuck, organic solvent is added and emulsifier, turn on agitator are mixed, leads to
Nitrogen 10min, obtains oil phase；
Water is added in reaction monomers acrylamide, acrylic acid, 2- acrylamide-2-methyl propane sulfonics and diallyl polyether
In aqueous solution is made, the pH for the sodium hydroxide solution regulation system for being 30% with mass concentration is 7.0~7.5, lead to nitrogen
20min obtains water phase；Wherein, shown in the following Formula IV of the structural formula of the diallyl polyether：
In Formula IV, EO is-OCH2CH2(epoxy ethyl), PO are-OCH (CH3)CH2(glycidyl)；0≤x<55,0≤
Y≤10,0≤z≤16 are 0 when x, y, z difference；
2) water phase obtained by step 1) is added dropwise in the oil phase that closed reactor is added, under 20 DEG C, 1500rpm speed conditions
Stir and lead to nitrogen 30min, make system emulsify after, be added initiator polymerize to get.
Reverse phase surface activating agent will be added in above-mentioned preparation method products obtained therefrom to get emulsion-type aqueous fracturing fluid drag reduction
Agent.
The type of each raw material and technical parameter are as shown in table 1 in embodiment 1-4 and comparative example.
The type and technical parameter of each raw material in 1 embodiment 1-4 of table
In table 1, the molecular formula of diallyl polyether (16EO) is：
The molecular formula of diallyl polyether (54.5EO) is：
The molecular formula of diallyl polyether (16EO10PO16EO) is：
Experimental example 1
This experimental example is detected the resistance reducing performance of drag reducer obtained by embodiment 1-4 and comparative example.Detection method is to incite somebody to action
Gained drag reducer is added in clear water, and it is 0.06%~0.15% to make the mass percentage of multiple copolymer, by testing clear
2 points of pressure difference before and after drag reducer is added in water, calculates drag reducing efficiency and carries out drag-reduction effect evaluation.The calculation formula of drag reducing efficiency is such as
Under：
In formula, Δ P0--- the frictional resistance pressure drop of pipeline section, MPa when unimplanted drag reducer；
ΔPDR--- the frictional resistance pressure drop of identical throughput rate lower tube section, MPa after injection drag reducer.
It is by the mass percentage of multiple copolymer in drag reducer addition clear water obtained by embodiment 1-4 and comparative example, is made
When 0.08%, testing result is as shown in Figure 1.
It will be seen from figure 1 that compared with comparative example, drag reducer is with the increase of discharge capacity, drag reducing efficiency obtained by embodiment 1-4
Increase obviously, up to 70%~75%.The experimental results showed that the linear structure of drag reducer of the invention in multiple copolymer
After middle introducing soft segment, drag reducing efficiency is significantly improved, and has excellent resistance reducing performance.
Experimental example 2
This experimental example can be detected the broken colloidality of drag reducer obtained by embodiment 1-4 and comparative example.Detection method is to incite somebody to action
Gained drag reducer is added in clear water, and it is 0.12% to make the mass percentage of multiple copolymer, obtains mixture；100g is weighed respectively
The ammonium persulfate solution that 0.5g mass concentrations are 10% is added in gained mixture, places at a set temperature, test system is apparent
The variation of viscosity, for evaluating brokenly colloidality energy.Test result is as shown in table 2.
The broken glue performance test results of 2 embodiment 1-4 of table and comparative example gained drag reducer
From table 2 it can be seen that compared with comparative example, the initial apparent ratio of viscosities of drag reducer obtained by embodiment 1-4 is larger, with
The apparent viscosity of time reduces fast.The experimental results showed that drawing in the linear structure of multiple copolymer in drag reducer of the invention
After entering soft segment, initial apparent viscosity increases, and breaks glue speed and accelerates, has excellent broken colloidality energy.
Claims (9)
1. a kind of acrylamide/sodium Acrylate multiple copolymer, it is characterised in that：The multiple copolymer contains Formulas I~formula IV institute
The four kinds of structural units shown：
In formula IV, EO is-OCH2CH2, PO is-OCH (CH3)CH2-；0≤x<55,0≤y≤10,0≤z≤16, x, y, z are different
When be 0.
2. a kind of preparation method of acrylamide/sodium Acrylate multiple copolymer as described in claim 1, it is characterised in that：
Include the following steps：
1) organic solvent is mixed with emulsifier, obtains oil phase；Reaction monomers are added to the water, aqueous solution is made, with sodium hydroxide tune
It is 7.0~7.5 to save pH, obtains water phase；The reaction monomers be acrylamide, acrylic acid, 2- acrylamide-2-methyl propane sulfonics and
Diallyl polyether；Wherein, shown in the following Formula IV of the structural formula of the diallyl polyether：
CH2=CH-CH2-(EO)x-(PO)y-(EO)z-O-CH2- CH=CH2
Formula IV；
In Formula IV, EO is-OCH2CH2, PO is-OCH (CH3)CH2-；0≤x<55,0≤y≤10,0≤z≤16, x, y, z are different
When be 0；
2) water phase obtained by step 1) is added in oil phase obtained by step 1), after stirring makes it emulsify, initiator is added and is polymerize,
To obtain the final product.
3. the preparation method of acrylamide/sodium Acrylate multiple copolymer according to claim 2, it is characterised in that：Step
It is rapid 1) in, the organic solvent is hexamethylene, kerosene, any one or combination in white oil.
4. the preparation method of acrylamide/sodium Acrylate multiple copolymer according to claim 2, it is characterised in that：Step
It is rapid 1) in, the emulsifier be sorbitan monostearate, sorbitan monooleate, polyoxyethylene shrink sorbierite
Any one in monoleate, hypermer 1083, hypermer 1031 or combination.
5. the preparation method of acrylamide/sodium Acrylate multiple copolymer according to claim 2, it is characterised in that：Step
In rapid 1) the described reaction monomers, acrylamide, acrylic acid, 2- acrylamide-2-methyl propane sulfonics and diallyl polyether matter
Amount is than being 100:8~30:5~30:1~15.
6. the preparation method of acrylamide/sodium Acrylate multiple copolymer according to claim 2, it is characterised in that：Step
It is rapid 2) in, when oil phase is added in water phase, the mass ratio of reaction monomers and organic solvent is 30~35:25~35.
7. the preparation method of acrylamide/sodium Acrylate multiple copolymer according to claim 2, it is characterised in that：Step
It is rapid 2) in, the initiator is the Redox Initiator body that ammonium persulfate or potassium peroxydisulfate are formed with sodium hydrogensulfite or sodium formaldehyde sulfoxylate
System.
8. a kind of emulsion-type aqueous fracturing fluid drag reducer, it is characterised in that：Contain acrylamide/propylene described in claim 1
Sour sodium multiple copolymer.
9. emulsion-type aqueous fracturing fluid drag reducer according to claim 8, it is characterised in that：Also contain reverse phase surface activity
Agent, the reverse phase surface activating agent are polyoxyethylene sorbitol acid anhydride trioleate, fat alcohol polyethylene ether, Nonyl pheno
Any one in ether or combination.
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