CN104087275B - A kind of high-temperature-resistant high-salt tiny gels granular profile control agent and its preparation method and application - Google Patents
A kind of high-temperature-resistant high-salt tiny gels granular profile control agent and its preparation method and application Download PDFInfo
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- CN104087275B CN104087275B CN201410331932.4A CN201410331932A CN104087275B CN 104087275 B CN104087275 B CN 104087275B CN 201410331932 A CN201410331932 A CN 201410331932A CN 104087275 B CN104087275 B CN 104087275B
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Abstract
Open a kind of high-temperature-resistant high-salt tiny gels granular profile control agent of the present invention and its preparation method and application.The preparation method of this tiny gels granule is to first pass through to add a certain proportion of modified starch, monomer A, monomer B, cross-linking agent, initiator and accelerator in reactor, after the polyreaction of these 6 kinds of components completes to form overall aqueous gel again the technical process such as drying, pulverizing, pelletize, screening and prepare.The application process that the present invention provides: a certain amount of tiny gels granule obtained in the present invention is joined in Bingham fluid, under static state and dynamic condition, gel particle all energy stable suspersions are without settling, and utilize to be pumped and more whole fluid injected stratum.A kind of high-temperature-resistant high-salt tiny gels granule provided by the present invention and application process thereof can improve being constructed into power and obtaining good deep profile controlling effect of gel particle greatly.
Description
Technical field
The present invention relates to a kind of high-temperature-resistant high-salt tiny gels granular profile control agent, relate to the system of this tiny gels granular profile control agent simultaneously
Preparation Method, and application new method in terms of strong water breakthrough passage in closure high temperature and high salt oil deposit.
Background technology
High temperature and high salt oil deposit generally exists in China, typically such as Zhongyuan Oil Field, and the oil such as Xinjiang, triumph, huge port, Ji Dong
The part oil district in field.These oil fields mostly have been enter into the middle and late stage of exploitation, and Cut of Oilfield is high, recovery percent of reserves is low, and remaining oil digs
Latent big, but owing to the feature of high temperature and high salt makes the increasing oil control water measure commonly used all lose efficacy.
Recovering the oil by Zhongyuan Oil Field as a example by the Wen Nan oil field of four factories, Wen Nan oil field is positioned at Dong-pu Depression central uplift belt literary composition and stays structure south
In secondary graben, it is an abnormal pressure, high temperature Complicated Fault-Block Hydrocarbon Reservoir, oil reservoir buried depth 2210～3800m, main force's oil
Pressure coefficient 1.2～1.8 under husky two times of layer, Sha Sanshang, Sha Sanzhong, sand three, formation temperature 92～140 DEG C, reservoir porosity
11.4%～21.6%, water surveys permeability (43.5～2289.5) × 10-3μm2, coefficient of permeability variation 0.7～0.98, permeability grade
5.06～64.83.Formation water salinity (21～34) × 104Mg/L, water type is CaCl2Type, belongs to typical high temperature and high salt heterogeneous body oil
Hide.The large area water logging at present of the preferable class main layer of this oil field producing status after waterflooding extraction for many years, comprehensive water cut
More than 80%, locally well aqueous up to 99%, and the two class layer water-driven difficulties that reservoir properties is poor.Open to improve oil field
Send out effect, in the urgent need to finding the profile control and water plugging technology being suitable for such oil reservoir.Conventional polyacrylamide adjusts stifled system application
Ceiling temperature is 90 DEG C, can not meet the job requirements in oil field the most completely.To this, in terms of profile control and water plugging, this factory is through deeply
Three kinds of profile control agents such as gel particle profile control agent, inorganic gel profile control agent, rubber grain profile control agent, these three class has been introduced after investigation
The profile control agent of type all can exist under high temperature and high salt environment steadily in the long term.But at the scene implementation process finds, inorganic gel profile control
Agent injection pressure when construction rises very fast, and follow-up plugging agent injects difficulty, and rubber grain profile control agent has heatproof, anti-shearing
Advantage, be the system that a kind of mechanical blockage is stronger, but in work progress, also show as that supercharging is fast, pressure is high, injection is difficult,
All can not meet the injection requirement of oil reservoir.And gel particle profile control agent disclosure satisfy that the injection requirement in Wen Nan oil field, well after profile control
Intake profile has clear improvement, and injection pressure rises, and main force's water accepting layer is effectively controlled, and new layer is started.And gel
Grain solves that Permeabilty agent enters behind stratum because dilute, shear, degrading, the various complexity reasons such as absorption cause does not becomes
The problems such as glue or gel-forming property variation, gel particle preparation is simple, easy construction, safety non-toxic, in the closure of strong water breakthrough passage
In there is the biggest prospect.But at the scene implementation process have also discovered many not enough: although gel particle has resistance to abnormal high temperature
Advantage, but suspension is poor, is easily deposited near borehole and results in blockage after entering pit shaft, affects normal construction, and construction terminates
Rear moisture content the most significantly rises so that construction effect duration is short, and intake profile test display is more uniform, this
Illustrating that gel particle is mainly blocked near wellbore zone, the remaining oil of low-permeability layer is preferably employed.
Therefore, in order to extend the effect duration of gel particle profile control, improve the effect of increasing production after profile control construction, develop injection efficiency
Earth formation deep can be entered well and the strong temperature resistance salt tolerant granular profile control agent of shut-off capacity seems extremely important.
Summary of the invention
It is an object of the invention to provide a kind of high-temperature-resistant high-salt tiny gels granular profile control agent, this profile control agent not only has high temperature resistance
The premium properties of high salt, and suspension is relatively good with stratum compatibility.Meanwhile, the present invention also provides for above-mentioned high temperature resistance
The preparation method of high salt tiny gels granular profile control agent and application new method.Utilize the high-temperature-resistant high-salt researched and developed in the present invention micro-
Thin gel particle profile control agent and heretofore described application process can obtain in high temperature and high salt oil deposit and the highest be constructed into power
With preferable deep profile controlling effect.
Concrete technical solution of the present invention is:
A kind of high-temperature-resistant high-salt tiny gels granular profile control agent, it is made up of following raw material: modified starch, monomer A, list
Body B, cross-linking agent, initiator, accelerator and water；Each raw material dosage is as follows: the mass fraction of modified starch is 4%～5%,
The mass fraction of monomer A is 3%～4%, and the mass fraction of monomer B is 1%～2%, the mass fraction of cross-linking agent be 0.04%～
0.06%, the mass fraction of initiator is 0.05%～0.15%, and the mass fraction of accelerator is 0.2%-0.4%, and other is water,
The mass fraction sum of each component is 100%；Described monomer A is acrylamide, and monomer B is 2-acrylamido-2-methyl
Propane sulfonic acid.
Preferably, being dissolved by the modified starch described in 5g in 95g water, the time of being completely dissolved is 45min, after being completely dissolved
Modified starch aqueous solution is homogeneous system；Described modified starch comes from the prosperous photochemical factory of Hebei Renqiu；Described cross-linking agent is
N, N ' methylene-bisacrylamide, described initiator is formed by potassium peroxydisulfate and sodium sulfite 2:1 in mass ratio
Mixture, described accelerator is sodium hydroxide.
The particle diameter of this tiny gels granular profile control agent can from main separation, particle diameter in >=10 μ m, preferred particle size range
Being 10 μm-53 μm, density is 1.21g/cm3。
The preparation method of a kind of high-temperature-resistant high-salt tiny gels granular profile control agent, comprises the following steps:
(1) being added the most lentamente to water by modified starch, be slowly added while stirring, starch to be modified continues after having added
Stirring, until fully dissolving, obtains starch solution；
(2) adding monomer A, monomer B, cross-linking agent, initiator and accelerator in starch solution, stirring, to dissolving, obtains
Reactant mixture；Described monomer A is acrylamide, and monomer B is 2-acrylamide-2-methylpro panesulfonic acid；
(3) reactant mixture is put in the calorstat more than 40 DEG C 5-10 hour and make it be polymerized, obtain overall gel, in half
Solid-state；
(4) particle diameter >=10 μm can be produced after obtained overall gel drying, pulverizing, pelletize, sieving technology process
High-temperature-resistant high-salt tiny gels granular profile control agent.
In preferred steps (1), described modified starch comes from the prosperous photochemical factory of Hebei Renqiu, and 5g modified starch is at 95g water
In the time that is completely dissolved be 45min, modified starch aqueous solution is homogeneous system.
In preferred steps (2), described cross-linking agent is N, N ' methylene-bisacrylamide, and described initiator is over cure
The mixture that acid potassium is formed with sodium sulfite 2:1 in mass ratio, described accelerator is sodium hydroxide.
The application process of a kind of high-temperature-resistant high-salt tiny gels granular profile control agent, is specially and is adjusted by high-temperature-resistant high-salt tiny gels granule
Cut open agent with Bingham fluid with the use of with water breakthrough passage strong in closure high temperature and high salt oil deposit.
Preferably, above-mentioned Bingham fluid is prepared by following steps:
(1) sodium bentonite that quality is 1.5g is added in 48.5g water, place 24 hours after being sufficiently stirred for, obtain sodium
Base bentonite aqueous solution；
(2) stabilizer that quality is 0.6g is added to 49.4g water, stir, obtain stabilizer aqueous solution；Described
Stabilizer is to be mixed by hydroxypropyl methyl cellulose and positive colloid 2:1 in mass ratio；
(3) stir after the stabilizer aqueous solution that sodium bentonite aqueous solution step (1) prepared and step (2) prepare
Uniformly, Bingham fluid is obtained.
Preferably, above-mentioned application process specifically includes following operation:
(1) note preposed attributives: inject described Bingham fluid in stratum；
(2) note principal piece plug: inject described high-temperature-resistant high-salt tiny gels granular profile control agent and described Bingham in stratum
The mixture of fluid, the mass fraction of wherein said high-temperature-resistant high-salt tiny gels granular profile control agent is 5%-10%, and surplus is institute
The Bingham fluid stated；Stop injecting when injection pressure is higher than 1.5 times of original formation pressure；
(3) rearmounted slug is noted: in stratum, inject described Bingham fluid；
(4) note formation water.
Said method can be used for temperature be 150 DEG C, salinity be all stratum containing strong water breakthrough passage of 300000mg/L.
The method have the benefit that:
(1) a kind of high-temperature-resistant high-salt tiny gels granule provided by the present invention has splendid viscoelasticity, migration in the earth formation
Ability is strong, easily enters earth formation deep, and the robust consistent under high temperature and high salt environment, so that the effect energy of deep profile controlling
Keep the long period.
(2) existing gel particle suspension difference and particle size difficulty are that gel particle is in maximum the lacking of application aspect with stratum compatibility
Falling into, suspension difference causes the dosing concentration can not be too high, and during on-the-spot application, gel particle concentration is below 0.5%, causes construction period
Long, particle size cross conference make the easy accumulated plugging of granule near wellbore zone, the undersized degradation that can make again gel particle.
High-temperature-resistant high-salt tiny gels granule provided by the present invention not only has a premium properties of high-temperature-resistant high-salt, and suspension and
Stratum compatibility is preferable, it is possible to obtain the highest is constructed into power and preferable deep profile controlling effect, can improve recovery ratio.
(3) preparation method of the present invention has and selects materials and consumption is reasonable, and preparation technology is simple, and low cost and other advantages can produce and provide
There are the high-temperature-resistant high-salt tiny gels granular profile control agent series of products of different Water absorption, absorption speed, particle radius and intensity.
(4), in application process provided by the present invention, tiny gels granule is whether under static conditions or dynamic condition
All can stable suspersion in Bingham fluid.
(5), in application process provided by the present invention, corresponding tiny gels particle size can be determined by the permeability on stratum
Scope, may determine that the performance of Bingham fluid by selected tiny gels particle size, and implementation process is flexible.
(6), in application process provided by the present invention, the mass concentration of tiny gels granule can be improved to more than 5%, can
To shorten greatly the engineering time and can improve and be constructed into power.
Accompanying drawing explanation
Fig. 1 illustrates the elastic modelling quantity of different-grain diameter tiny gels granule；
Fig. 2 illustrates the loss modulus of different-grain diameter tiny gels granule；
Fig. 3 illustrates the rheological curve of Bingham fluid；
Fig. 4 is dynamic physical modeling experiments device schematic diagram；
Fig. 5 illustrates the tiny gels granule of 270 mesh (53 μm) injection pressure under different quality mark；
Fig. 6 illustrates the tiny gels granule of 325 mesh (44 μm) injection pressure under different quality mark；
Fig. 7 illustrates the tiny gels granule of 400 mesh (37 μm) injection pressure under different quality mark；
Fig. 8 illustrate mass fraction be 10% particle diameter be the tiny gels granule migration curve in the earth formation of 325 mesh (44 μm).
Detailed description of the invention
With specific embodiment, the present invention is elaborated below in conjunction with the accompanying drawings, but the invention is not restricted to following embodiment.
One, the preparation of high-temperature-resistant high-salt tiny gels granular profile control agent
The modified starch of 50g is added in the water of 898g, after fully dissolving, add the 2-acrylamido-2-methyl of 15g
Propane sulfonic acid (AMPS), the acrylamide (AM) of 35g, the N of 0.5g, N ' methylene-bisacrylamide, the sodium hydroxide of 3g,
The potassium persulfate of 0.6g and the sodium sulfite of 0.3g, until solution stirring fully after seal, put into 40 DEG C of calorstats 10 hours
Rear taking-up, solution has become overall block gel the most.Take out block overall gel carry out drying, pulverize, the work such as pelletize
Skill make particle diameter be 270 mesh (53 μm), 325 mesh (44 μm), 400 mesh (37 μm), 550 mesh (25 μm), 800 mesh (15 μm) and
The tiny gels granule of 1250 mesh (10 μm).
Two, the static properties test of high-temperature-resistant high-salt tiny gels granular profile control agent
The gel particle of different-grain diameter prepared in above-mentioned steps is put into homemade salinity is 30 × 104In the saline of mg/L
After be held in the calorstat of 150 DEG C and investigate its stability.The static evaluation experimental result of tiny gels granular profile control agent is shown in Table
1, tiny gels granule the most provided by the present invention has splendid temperature resistance salt resistant character.
Table 1
By the tiny gels granule of different-grain diameter prepared in above-mentioned steps 150 DEG C through salinity be 30 × 104Mg/L's
Saline soak tests its viscoelasticity after 60 days.Test instrunment is the flat plate model of RS-600 flow graph.Test result such as Fig. 1 and
Shown in Fig. 2, Fig. 1 is the elastic modelling quantity of the tiny gels granule of different-grain diameter, and Fig. 2 is the tiny gels granule of different-grain diameter
Loss modulus.It is recognized that while the elastic modelling quantity of tiny gels granule and loss modulus are all along with grain size from Fig. 1 and Fig. 2
Reduction and reduce, but even if tiny gels granule also can keep the highest viscoelastic under minimum grain size size 1250 mesh (10 μm)
Property, this illustrate different-grain diameter provided by the present invention gel particle 150 DEG C through salinity be 30 × 104The saline of mg/L
Remain high viscoelasticity after soaking 60 days, this is that tiny gels granule is migrated the most smoothly to earth formation deep and has the highest
The physical basis of plugging strength.
Three, the research and development of Bingham fluid and performance test thereof
The salinity of test water is 30 × 104mg/L.The sodium bentonite that 1.5g particle diameter is 1250 mesh (10 μm) is added extremely
In the water of 48.5g, stirring fully, obtains sodium bentonite solution.Will be by 0.4g hydroxypropyl methyl cellulose and 0.2g positive colloid
The stabilizer formed adds to 49.6g water, and stirring fully, obtains stabiliser solution.By sodium bentonite solution with stable
Agent solution mixes, and is heretofore described Bingham fluid after stirring.The viscosity of the Bingham fluid of gained is
30.3mPa.s, density is 1.08g/cm3.RS-600 flow graph is utilized to survey the rheological curve of Bingham fluid, as shown in Figure 3.
According to the research of nineteen ninety-five Daqing Petroleum Institute Lee rainbow et al., can occur suspending not sink in the fluid of band surrender application
Phenomenon, the critical condition that granule suspends in Bingham fluid is:
ρ in formulasFor the density (after expansion) of gel particle, d is the particle diameter (after expansion) of gel particle, τoBending for suspension
Taking stress, ρ is the density of suspension.As can be known from Fig. 3, according to curve-fitting results, the yield value of fluid is 0.019.Profit
Bingham fluid provided by the present invention can be calculated with formula (1) can suspend the gel particle that particle diameter is 150 μm.
And the gel particle particle diameter provided in the present invention is respectively less than 150 μm, therefore the Bingham fluid provided in the present invention is permissible
Tiny gels granule provided in the suspension present invention.
Being added by the tiny gels granule of 270 mesh (53 μm) of 5g in the Bingham fluid of 45g, after stirring, gained mixes
The gross mass of compound is 50g, and density is 1.13g/cm3.Take upper part 20mL of fluid mixture after standing 30min, survey it
Quality is 22.6g, and density is 1.13g/cm3, the quality of fluid mixture lower part is 27.4g, and density is 1.13g/cm3, survey
Bingham fluid in the examination description of test present invention can suspend tiny gels granule prepared in the present invention uniformly.
Four, injection efficiency and the transfer ability of tiny gels granule is tested
Dynamic physical modeling experiments condition is with Wen Nan oil field as foundation, and the formation temperature in Wen Nan oil field is 92～140 DEG C, and water is surveyed and oozed
Rate (43.5～2289.5) × 10 thoroughly-3μm2, formation water salinity (21～34) × 104mg/L.Laboratory experiment temperature is 140 DEG C, simulation
Water salinity is 300000mg/L.Physical simulation experiment device as shown in Figure 4, a length of 1m of fill out sand tube, diameter in test
For 2.5cm, permeability is 2200mD, and porosity is 37%, and pore volume is 217cm3.Can by the permeability of fill out sand tube
With the gel particle that initial option is corresponding.Select particle diameter be 270 mesh (53 μm), 325 mesh (44 μm), three kinds of 400 mesh (37 μm)
Granulated gel is as experimental subject.
It is 270 mesh (53 μm), 325 mesh (44 μm), three kinds of granulated gels of 400 mesh (37 μm) by particle diameter prepared in the present invention
Add in the Bingham fluid researched and developed to the present invention, form the fluid mixture of different quality mark.Utilize dynamic physical
The injection efficiency of analogue experiment installation test these three tiny gels granule.Test process keeps the injection rate of tiny gels granule
Constant, it is 0.2PV, i.e. 43.6cm3, being converted into quality is 52.7g.Injection rate in test process is 0.2mL/min.
The volume of injection fluid is changed by adjusting tiny gels granule mass fraction in Bingham fluid.Test result such as figure
5, shown in Fig. 6, Fig. 7 and Fig. 8.Fig. 5 be particle diameter be that the tiny gels granule of 270 mesh (53 μm) is under different quality mark
Inject curve.Fig. 6 be particle diameter be the tiny gels granule of 325 mesh (44 μm) injection curve under different quality mark.Fig. 7
For tiny gels granule that particle diameter is 400 mesh (37 μm) the injection curve under different quality mark.Knowable to Fig. 5-7, this
Tiny gels granule provided in bright is relatively low with the injection pressure of Bingham fluid mixture, can enter stratum, explanation smoothly
Tiny gels granule provided in the present invention has good injection.Fig. 8 be mass fraction be 10%, particle diameter be 325 mesh
The tiny gels granule of (44 μm) migration curve in the earth formation, as can be known from Fig. 8, tiny gels granule can progressively be migrated to ground
Layer depth portion, can play the effect of earth formation deep fluid diversion.This illustrates that tiny gels granule provided by the present invention has in the earth formation
There is splendid transfer ability.Therefore, the present invention is researched and developed tiny gels granule and application process thereof can meet high temperature and high salt oil deposit
The requirement of deep profile controlling.
Claims (7)
1. a high-temperature-resistant high-salt tiny gels granular profile control agent, it is characterised in that be made up of following raw material: modified starch,
Monomer A, monomer B, cross-linking agent, initiator, accelerator and water；Each raw material dosage is as follows: the mass fraction of modified starch is
4%～5%, the mass fraction of monomer A is 3%～4%, and the mass fraction of monomer B is 1%～2%, and the quality of cross-linking agent is divided
Number is 0.04%～0.06%, and the mass fraction of initiator is 0.05%～0.15%, and the mass fraction of accelerator is 0.2%-0.4%,
Other is water, and the mass fraction sum of each component is 100%；Described monomer A is acrylamide, and monomer B is 2-acrylamide
Base-2-methyl propane sulfonic acid；Being dissolved in 95g water by modified starch described in 5g, the time of being completely dissolved is 45min, the most molten
Modified starch aqueous solution after solution is homogeneous system；Described cross-linking agent is N, N ' methylene-bisacrylamide, and described draws
Sending out the mixture that agent is formed with sodium sulfite 2:1 in mass ratio by potassium peroxydisulfate, described accelerator is sodium hydroxide.
A kind of high-temperature-resistant high-salt tiny gels granular profile control agent the most according to claim 1, it is characterised in that: this is fine solidifying
The particle size range of glue granular profile control agent is 10 μm-53 μm, and density is 1.21g/cm3。
3. the preparation method of high-temperature-resistant high-salt tiny gels granular profile control agent as claimed in claim 1, it is characterised in that include with
Lower step:
(1) being added the most lentamente to water by modified starch, be slowly added while stirring, starch to be modified continues after having added
Stirring, until fully dissolving, obtains starch solution；
(2) adding monomer A, monomer B, cross-linking agent, initiator and accelerator in starch solution, stirring, to dissolving, obtains
Reactant mixture；Described monomer A is acrylamide, and monomer B is 2-acrylamide-2-methylpro panesulfonic acid；
(3) reactant mixture is put in the calorstat more than 40 DEG C 5-10 hour and make it be polymerized, obtain overall gel, in half
Solid-state；
(4) fine by producing high-temperature-resistant high-salt after obtained overall gel drying, pulverizing, pelletize, sieving technology process
Gel particle profile control agent.
The preparation method of a kind of high-temperature-resistant high-salt tiny gels granular profile control agent the most according to claim 3, it is characterised in that:
In step (1), described modified starch comes from the prosperous photochemical factory of Hebei Renqiu, complete in 95g water of 5g modified starch
Dissolution time is 45min, and modified starch aqueous solution is homogeneous system.
The preparation method of a kind of high-temperature-resistant high-salt tiny gels granular profile control agent the most according to claim 3, it is characterised in that:
In step (2), described cross-linking agent is N, N ' methylene-bisacrylamide, and described initiator is that potassium peroxydisulfate is with sub-
The mixture that sodium bisulfate 2:1 in mass ratio is formed, described accelerator is sodium hydroxide.
6. the application process of a high-temperature-resistant high-salt tiny gels granular profile control agent, it is characterised in that: described in claim 1
High-temperature-resistant high-salt tiny gels granular profile control agent leads to the use of with water breakthrough strong in closure high temperature and high salt oil deposit with Bingham fluid
Road；
Described Bingham fluid is prepared by following steps:
(1) sodium bentonite that quality is 1.5g is added in 48.5g water, place 24 hours after being sufficiently stirred for, obtain sodium
Base bentonite aqueous solution；
(2) stabilizer that quality is 0.6g is added to 49.4g water, stir, obtain stabilizer aqueous solution；Described
Stabilizer is to be mixed by hydroxypropyl methyl cellulose and positive colloid 2:1 in mass ratio；
(3) stir after the stabilizer aqueous solution that sodium bentonite aqueous solution step (1) prepared and step (2) prepare
Uniformly, Bingham fluid is obtained；
Described application process specifically includes following operation:
(1) note preposed attributives: inject described Bingham fluid in stratum；
(2) note principal piece plug: inject described high-temperature-resistant high-salt tiny gels granular profile control agent and described Bingham in stratum
The mixture of fluid, the mass fraction of wherein said high-temperature-resistant high-salt tiny gels granular profile control agent is 5%-10%, and surplus is institute
The Bingham fluid stated；Stop injecting when injection pressure is higher than 1.5 times of original formation pressure；
(3) rearmounted slug is noted: in stratum, inject described Bingham fluid；
(4) note formation water.
The application process of a kind of high-temperature-resistant high-salt tiny gels granular profile control agent the most according to claim 6, it is characterised in that:
The method can be used for temperature be 150 DEG C, salinity be all stratum containing strong water breakthrough passage of 300000mg/L.
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