CN109097018A - Micro Heterogeneous profile control agent and preparation method thereof - Google Patents
Micro Heterogeneous profile control agent and preparation method thereof Download PDFInfo
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Abstract
The present invention provides a kind of Micro Heterogeneous profile control agent and preparation method thereof, carries out polymerization reaction by heat and salinity tolerance monomer, major pharmaceutical, initiator, crosslinking agent, emulsifier, auxiliary agent, decentralized medium and water and forms；Wherein the weight percent of heat and salinity tolerance monomer is 1 to 5%, the weight percent of major pharmaceutical is 10 to 30%, the weight percent of initiator is 0.1 to 0.3%, the weight percent of crosslinking agent is 0.05 to 0.1%, the weight percent of emulsifier is 10 to 12%, the weight percent of decentralized medium is 45 to 65%, the weight percent of auxiliary agent is 0.1 to 1%, remaining is water；The Micro Heterogeneous profile control agent delays that swollen effect is good, expansion multiple is big；With excellent heat and salt resistance, chemical stability and injection；Deep migration and delay can be realized in oil reservoir, increases macropore or high permeable strip filtrational resistance, improves injection pressure, subsequent oil displacement agent is promoted to be redirected into middle less permeable layer, expand swept volume and improves recovery ratio, improve high water cut oil field recovery ratio.
Description
Technical field
The present invention relates to a kind of Micro Heterogeneous profile control agents and preparation method thereof.
Background technique
Currently, waterflooding extraction mode is taken in oil field mostly both at home and abroad, due to reservoir itself heterogeneity and long-term high-strength
Degree injection water washes away and destruction, causes oil reservoir high permeability zone permeability and reservoir heterogeneity to further increase, causes to infuse
Enter water or oil displacement agent is advanced by leaps and bounds along predominant pathway, forms inefficient or inefficient cycle, it is final to reduce less permeable layer wave and efficiency in oil reservoir
And recovery ratio.Therefore, high water-cut development period oil deposit deep part fluid diversion technology has become the key technology for improving recovery ratio.
Particulate species Micro Heterogeneous profile control agent has " stifled very much not block up small " seepage characteristic, Micro Heterogeneous compared with polymer solution
Profile control agent and carrying liquid water generate " tune " and " drive " coordinating effect, can obtain preferable oil increasing precipitation effect.In addition, microcosmic non-equal
Matter profile control agent, which also has, delays swollen effect, and deep migration and expansion plugging effect may be implemented.Therefore, Micro Heterogeneous profile control agent exists
Effect in terms of raising high water-cut reservoir recovery ratio is more and more taken seriously, and has broad prospect of application.Existing Micro Heterogeneous
Profile control agent expansion multiple generally 5 or so, has a certain gap, it would be highly desirable to which exploitation delays the swollen time more away from mining site production actual demand
Micro Heterogeneous profile control agent product long, expansion multiple is bigger.
Summary of the invention
It is a primary object of the present invention to overcome disadvantages mentioned above of the existing technology, and provide a kind of Micro Heterogeneous tune
Agent and its preparation method are driven, formula and process conditions are reasonable, effectively improve Micro Heterogeneous profile control agent and delay swollen time and expansion multiple.
The purpose of the present invention is implemented by the following technical solutions.
Micro Heterogeneous profile control agent of the present invention, which is characterized in that it is by heat and salinity tolerance monomer, major pharmaceutical, initiator, friendship
Connection agent, emulsifier, auxiliary agent, decentralized medium and water carry out polymerization reaction and form；The wherein weight percent of heat and salinity tolerance monomer
Weight percent for 1 to 5%, major pharmaceutical is 10 to 30%, the weight percent of initiator is 0.1 to 0.3%, crosslinking agent
Weight percent is 0.05 to 0.1%, the weight percent of emulsifier is 10 to 12%, the weight percent of decentralized medium is 45
Weight percent to 65%, auxiliary agent is 0.1 to 1%, remaining is water.
Micro Heterogeneous profile control agent above-mentioned, wherein the heat and salinity tolerance monomer is 2- acrylamido -2- methyl-prop sulphur
Sour (AMPS)；The major pharmaceutical is the mixture of acrylamide (AM), α-methylstyrene (α-MSt) and acrylic acid (AA),
Wherein the weight percent of acrylamide (AM) is 80 to 90%, the weight percent of α-methylstyrene (α-MSt) be 5 to
7%, acrylic acid (AA) is surplus；The auxiliary agent is sodium hydroxide (NaOH)；The initiator is ammonium persulfate (APS) and sulfurous
Sour sodium (Na2SO3) mixture, wherein ammonium persulfate (APS), sodium sulfite (Na2SO3) weight ratio be 2:1；The friendship
Connection agent is N,N methylene bis acrylamide (MBA)；The emulsifier is the mixed of tween (Tween) -80 and this disk (Span) -80
Object is closed, wherein the weight ratio of Tween 80 and span 80 is 10:13；The decentralized medium is atoleine；The water be go from
Sub- water.
The preparation method of Micro Heterogeneous profile control agent of the invention, which comprises the following steps:
(1) match production of hybrid seeds liquid
Oily phase: atoleine is successively weighed according to formula rate, Tween-80 and Span-80, which are placed in small beaker, to be stirred
Uniformly；
Water phase: separately taking a small beaker, and deionized water is successively weighed according to formula rate, heat and salinity tolerance monomer, major pharmaceutical, is helped
Agent (NaOH) and crosslinking agent and being placed in beaker dissolves；
Initiator: a certain amount of deionized-distilled water is taken to dissolve a certain amount of ammonium persulfate (APS) and sodium sulfite respectively
(Na2SO3) in two small beakers, it is sealed with preservative film spare；
Oily phase kind liquid is added in four-neck flask and is stirred, while water phase kind liquid is instilled dropwise in oily phase kind liquid, stirring is pre-
It is started to warm up after emulsification 30min, until when certain temperature, the nitrogen charging gas shielded 30min into four-neck flask, while being dripped dropwise with needle tubing
Enter above-mentioned initiator, reacts 1h；
(2) dropping liquid is prepared
Oily phase: atoleine is successively weighed according to formula rate, Tween-80 and Span-80, which are placed in small beaker, to be stirred
Uniformly；
Water phase: separately taking a small beaker, and deionized water is successively weighed according to formula rate, heat and salinity tolerance monomer, major pharmaceutical, is helped
Agent (NaOH) and crosslinking agent and being placed in beaker dissolves；
Initiator: a certain amount of deionized-distilled water is taken to dissolve a certain amount of ammonium persulfate (APS) and sodium sulfite respectively
(Na2SO3) in two small beakers, it is sealed with preservative film spare；
Oily phase dropping liquid is placed in a beaker stirring, while water phase dropping liquid is instilled dropwise in oily phase dropping liquid, stirs pre-emulsification
30min。
(3) polymerization reaction
After kind of liquid reacts 1 hour, the dropping liquid after pre-emulsification 30min is poured into constant pressure titration funnel, constant pressure is titrated
Funnel is placed in four-neck flask, and dropping liquid is instilled dropwise in the four-neck flask for filling kind of liquid, while nitrogen charging gas shielded 30min, and
The initiator of dropping liquid is instilled in four-neck flask dropwise respectively with needle tubing.Then each neck mouth is blocked, reacts four hours, obtains
Finished product.
The preparation method of Micro Heterogeneous profile control agent above-mentioned, wherein the weight percent of the heat and salinity tolerance monomer is 1
Weight percent to 5%, major pharmaceutical is 10 to 30%, the weight percent of initiator is 0.1 to 0.3%, the weight of crosslinking agent
Amount percentage be 0.05 to 0.1%, the weight percent of emulsifier is 10 to 12%, the weight percent of decentralized medium be 45 to
65%, the weight percent of auxiliary agent is 0.1 to 1%, remaining is deionized water.
The preparation method of Micro Heterogeneous profile control agent above-mentioned, wherein the heat and salinity tolerance monomer is 2- acrylamido-
2- methyl propane sulfonic acid (AMPS)；The major pharmaceutical be acrylamide (AM), 2- acrylamide-2-methylpro panesulfonic acid (AMPS),
The mixture of α-methylstyrene (α-MSt) and acrylic acid (AA), wherein the weight percent of acrylamide (AM) be 80 to
90%, the weight percent of α-methylstyrene (α-MSt) is 5 to 7%, and acrylic acid (AA) is surplus；The auxiliary agent is hydrogen-oxygen
Change sodium (NaOH)；The initiator is ammonium persulfate (APS) and sodium sulfite (Na2SO3) mixture, wherein ammonium persulfate
(APS), sodium sulfite (Na2SO3) weight ratio be 2:1；The crosslinking agent is N,N methylene bis acrylamide (MBA)；Institute
The mixture that emulsifier is tween (Tween) -80 and this disk (Span) -80 is stated, wherein the weight ratio of Tween 80 and span 80
For 10:13；The decentralized medium is atoleine；The water is deionized water.
Micro Heterogeneous profile control agent of the present invention and its preparation method the utility model has the advantages that the Micro Heterogeneous profile control agent, which has, delays swollen effect
Effect that fruit is good, expansion multiple is big and expansion period is long；And there is excellent heat and salt resistance, chemical stability and injection
Property；Deep migration and delay can be realized in oil reservoir, increases macropore or high permeable strip filtrational resistance, improve injection pressure
Power promotes subsequent oil displacement agent to be redirected into middle less permeable layer, expands swept volume and improves recovery ratio, improves for high water cut oil field
Recovery ratio measure provides technical guarantee.
Detailed description of the invention
Fig. 1 is Micro Heterogeneous transfer drive agent material infrared spectrum curve figure of the present invention.
Fig. 2 is Micro Heterogeneous profile control agent median particle size of the present invention and hydration time relational graph.
Fig. 3 is Micro Heterogeneous profile control agent expansion multiple of the present invention and hydration time relational graph.
In figure: microballoon 1 indicates that the Micro Heterogeneous profile control agent of this indoor synthesis, microballoon 2, microballoon 3 indicate normal at this stage
The Micro Heterogeneous profile control agent of rule.
Subordinate list explanation
Table 1 is the orthogonal design table of optimization of C/C composites of the present invention.
Table 2 is the specific formula composition of 9 groups of orthogonal tests of the present invention.
Table 3 is Micro Heterogeneous profile control agent partial size of the present invention with the variation of hydration time, reflects that it is swollen in water flooding
Swollen performance.
Table 4 is that Micro Heterogeneous profile control agent of the present invention delays swollen test result in rock core, reflects it in porous media
Expansion plugging effect.
Table 5 is that Micro Heterogeneous profile control agent of the present invention delays the swollen transmission migration effect blocked when testing in rock core.
Specific embodiment
The following describes the present invention in detail with reference to the accompanying drawings and specific embodiments.
1, Micro Heterogeneous profile control agent of the present invention is by heat and salinity tolerance monomer, major pharmaceutical, initiator, crosslinking agent, emulsification
Agent, auxiliary agent, decentralized medium and water carry out polymerization reaction and form；Wherein the weight percent of heat and salinity tolerance monomer be 1 to 5%,
The weight percent of major pharmaceutical is 10 to 30%, the weight percent of initiator is 0.1 to 0.3%, the weight percent of crosslinking agent
Than be 10 to 12% for the weight percent of 0.05 to 0.1%, emulsifier, the weight percent of decentralized medium is 45 to 65%,
The weight percent of auxiliary agent is 0.1 to 1%, remaining is water.Wherein, which is 2- acrylamido -2- methyl
Propane sulfonic acid (AMPS)；The major pharmaceutical is the mixing of acrylamide (AM), α-methylstyrene (α-MSt) and acrylic acid (AA)
Object, wherein the weight percent of acrylamide (AM) is 80 to 90%, and the weight percent of α-methylstyrene (α-MSt) is 5
To 7%, acrylic acid (AA) is surplus；The auxiliary agent is sodium hydroxide (NaOH)；The initiator is ammonium persulfate (APS) and sulfurous acid
Sodium (Na2SO3) mixture, wherein ammonium persulfate (APS), sodium sulfite (Na2SO3) weight ratio be 2:1；The crosslinking agent
For N,N methylene bis acrylamide (MBA)；The emulsifier is the mixture of tween (Tween) -80 and this disk (Span) -80,
Wherein the weight ratio of Tween 80 and span 80 is 10:13；The decentralized medium is atoleine；The water is deionized water.
The preparation method of Micro Heterogeneous profile control agent of the invention comprising following steps:
(1) match production of hybrid seeds liquid
Oily phase: atoleine is successively weighed according to formula rate, Tween-80 and Span-80, which are placed in small beaker, to be stirred
Uniformly；
Water phase: separately taking a small beaker, and deionized water is successively weighed according to formula rate, heat and salinity tolerance monomer, major pharmaceutical, is helped
Agent (NaOH) and crosslinking agent and being placed in beaker dissolves；
Initiator: a certain amount of deionized-distilled water is taken to dissolve a certain amount of ammonium persulfate (APS) and sodium sulfite respectively
(Na2SO3) in two small beakers, it is sealed with preservative film spare；
Oily phase kind liquid is added in four-neck flask and is stirred, while water phase kind liquid is instilled dropwise in oily phase kind liquid, stirring is pre-
It is started to warm up after emulsification 30min, until when certain temperature, the nitrogen charging gas shielded 30min into four-neck flask, while being dripped dropwise with needle tubing
Enter above-mentioned initiator, reacts 1h；
(2) dropping liquid is prepared
Oily phase: atoleine is successively weighed according to formula rate, Tween-80 and Span-80, which are placed in small beaker, to be stirred
Uniformly；
Water phase: separately taking a small beaker, and deionized water is successively weighed according to formula rate, heat and salinity tolerance monomer, major pharmaceutical, is helped
Agent (NaOH) and crosslinking agent and being placed in beaker dissolves；
Initiator: a certain amount of deionized-distilled water is taken to dissolve a certain amount of ammonium persulfate (APS) and sodium sulfite respectively
(Na2SO3) in two small beakers, it is sealed with preservative film spare；
Oily phase dropping liquid is placed in a beaker stirring, while water phase dropping liquid is instilled dropwise in oily phase dropping liquid, stirs pre-emulsification
30min。
(3) polymerization reaction
After kind of liquid reacts 1 hour, the dropping liquid after pre-emulsification 30min is poured into constant pressure titration funnel, constant pressure is titrated
Funnel is placed in four-neck flask, and dropping liquid is instilled dropwise in the four-neck flask for filling kind of liquid, while nitrogen charging gas shielded 30min, and
The initiator of dropping liquid is instilled in four-neck flask dropwise respectively with needle tubing.Then each neck mouth is blocked, reacts four hours, obtains
Finished product.
The preparation method of Micro Heterogeneous profile control agent of the invention, wherein the weight percent of the heat and salinity tolerance monomer is 1
Weight percent to 5%, major pharmaceutical is 10 to 30%, the weight percent of initiator is 0.1 to 0.3%, the weight of crosslinking agent
Amount percentage be 0.05 to 0.1%, the weight percent of emulsifier is 10 to 12%, the weight percent of decentralized medium be 45 to
65%, the weight percent of auxiliary agent is 0.1 to 1%, remaining is deionized water.The heat and salinity tolerance monomer is 2- acrylamido-
2- methyl propane sulfonic acid (AMPS)；The major pharmaceutical is acrylamide (AM), 2- acrylamide-2-methylpro panesulfonic acid (AMPS), α-
The mixture of methyl styrene (α-MSt) and acrylic acid (AA), wherein the weight percent of acrylamide (AM) be 80 to
90%, the weight percent of α-methylstyrene (α-MSt) is 5 to 7%, and acrylic acid (AA) is surplus；The auxiliary agent is hydroxide
Sodium (NaOH)；The initiator is ammonium persulfate (APS) and sodium sulfite (Na2SO3) mixture, wherein ammonium persulfate (APS),
Sodium sulfite (Na2SO3) weight ratio be 2:1；The crosslinking agent is N,N methylene bis acrylamide (MBA)；The emulsifier is
The mixture of tween (Tween) -80 and this disk (Span) -80, wherein the weight ratio of Tween 80 and span 80 is 10:13；It should
Decentralized medium is atoleine；The water is deionized water.
Micro Heterogeneous profile control agent properties of product characterization of the present invention.
(1) infrared absorption spectrum
1. copolymer Micro Heterogeneous profile control agent purifies
Lotion is equal to " 1:10 " ratio with volume ratio to be put into dehydrated alcohol, is sufficiently stirred and is demulsified, in bottom of the beaker
Portion generates a large amount of white flocculent deposits.To remove Micro Heterogeneous profile control agent adsorption surfactant, repeatedly distilled
Water washing obtains filter cake after suction filtration.Again with the ethanol washing of volume ratio " 1:5 ", suction filtration, filter cake natural air drying is obtained, is obtained white
Color powder.So as to subsequent infrared test.
Using orthogonal test method.Selected AMPS, emulsifier, initiator and temperature etc. are factor of evaluation, select 4 factors 3
Horizontal quadrature tests table experiment arrangement, is shown in Table 1, formula composition is shown in Table 2.
2. examination of infrared spectrum
Using 750 fourier infrared analysis tester of Nicolet Magna-IR, the Micro Heterogeneous transfer drive that will have been purified
Agent is tested with the finely ground compacting film forming of potassium bromide powder.
Using α-methylstyrene (α-MSt) and water-soluble monomer 2- acrylamide-2-methylpro panesulfonic acid (AMPS) and
Acrylamide (AM) and acrylic acid (AA) is quarternary copolymerized obtains Micro Heterogeneous profile control agent, then carries out examination of infrared spectrum point
Analysis.
(2) Micro Heterogeneous profile control agent particle diameter distribution
5000mg/L Micro Heterogeneous transfer drive agent solution is prepared using oil field simulated injection water, is placed in 65 DEG C of incubators,
Regular sample detection.10min~20min is first stirred before detection, then is drawn a small amount of sample with injector for medical purpose and dripped on glass slide,
Biomicroscope periodic observation Micro Heterogeneous profile control agent form and size are used later, determine Micro Heterogeneous profile control agent appearance
Size and hydration time relationship, statistics Micro Heterogeneous profile control agent expansion front and back particle diameter distribution.
(3) Micro Heterogeneous profile control agent delays swollen effect under static conditions
Micro Heterogeneous profile control agent prepare and storing apparatus equipment include HJ-6 type bull magnetic stirring apparatus, electronic balance,
III A type insulating box of beaker, test tube and HW- etc., Micro Heterogeneous profile control agent must carry out droplet measurement or rock core stream after preparing immediately
Dynamic property experiment, is influenced with reducing standing time to Micro Heterogeneous profile control agent hydration swelling effect bring.Using special optics difficult to understand
Instrument company produces BDS400 inverted biologic microscope observation Micro Heterogeneous profile control agent mode of appearance and size distribution and its becomes
Law.
It takes and is widely used on this method synthesis Micro Heterogeneous profile control agent sample " Micro Heterogeneous profile control agent 1 " and oil field
Micro Heterogeneous profile control agent sample " Micro Heterogeneous profile control agent 2 " and " Micro Heterogeneous profile control agent 3 " carry out delaying swollen performance test,
Each sample test initial stage, for 24 hours, 6 moment such as 72h, 120h, 196h and 240h, determine Micro Heterogeneous profile control agent partial size and
Particle diameter distribution and time relationship.
(4) Micro Heterogeneous profile control agent delays swollen effect in rock core
Rock core displacement test equipment mainly includes constant-flux pump, pressure sensor, hand pump and intermediate receptacle etc..Except constant-flux pump
Outside hand pump, other parts are placed in 65 DEG C of insulating boxs of Bohai Sea reservoir temperature.
Micro Heterogeneous profile control agent delays swollen capacity experimental step: it is microcosmic non-equal 1. to prepare design concentration using oilfield injection water
Micro Heterogeneous transfer drive agent solution is packed into real-time stirred type intermediate receptacle by matter transfer drive agent solution, keeps stirring in intermediate receptacle
It mixes paddle and is constantly in working condition, precipitated to avoid Micro Heterogeneous profile control agent；2. by constant-flux pump, intermediate receptacle and rock core
Clamper is connected with pipeline, forms an injection and extraction system, except clamper is placed under the conditions of reservoir temperature in insulating box, other portions
Part is placed in outside incubator；3. improving clamper ring pressure pressure to 5MPa or more, it is ensured that ring pressure pressure be greater than injection pressure 1MPa with
On；4. starting constant-flux pump, it is microcosmic non-to design PV (rock pore volume multiple) number with 3mL/min~6mL/min ultraspeed
Homogeneous transfer drive agent solution injects rock core, termination of pumping；5. rock core is taken out from clamper, rock core injection end 1.5cm~3.0cm long is cut away
Degree (eliminates Micro Heterogeneous profile control agent in " bridge blinding " effect that rock core end face near zone is detained and is formed), then by rock core by original
State puts back to clamper；6. carrying out water drive with normal injection rate 0.3mL/min, record initial stage water drive injects pressure difference δ when stablizing
P1；7. clamper remains in insulating box, subsequent waterflooding is carried out, record injection pressure difference after water drive is stablized.
Micro Heterogeneous profile control agent delays swollen merit rating step: 1. from the established water drive of third step " injection pressure difference and speed
The corresponding injection pressure difference δ P of injection rate 0.3mL/min or 0.5mL/min is discovered and seized on relation curve "0, Micro Heterogeneous profile control agent envelope
Stifled rate: η=(δ P0-δP)/δP；2. comparing different manufacturers or different formulations composition or different synthesis technology Micro Heterogeneous transfer drives
Agent sealing ratiod determines that the heterogeneous profile control agent of diverse microcosmic delays swollen effect and performance relative superior or inferior degree in rock core hole.
(5) Micro Heterogeneous profile control agent plugging effect is tested
To rock core (homogeneous rock core, Kg=500 × 10-3μm2~3000 × 10-3μm2, inject water) in injection 1.2PV it is microcosmic
Heterogeneous transfer drive agent solution (Micro Heterogeneous profile control agent 1, Micro Heterogeneous profile control agent 2 and Micro Heterogeneous profile control agent 3, concentration
0.3%), delay swollen 8d, subsequent waterflooding to pressure is stablized.
(6) Micro Heterogeneous profile control agent transmission migration aptitude tests
To rock core (homogeneous rock core, Kg=3000 × 10-3μm2, inject water) in inject 1.2PV Micro Heterogeneous profile control agent
(Micro Heterogeneous profile control agent 1, Micro Heterogeneous profile control agent 2 and Micro Heterogeneous profile control agent 3, concentration 0.3%), records each survey
Pressure point pressure change.Delay swollen 8d, subsequent waterflooding to pressure is stablized, and records pressure tap pressure change again.
Interpretation of result
1, Micro Heterogeneous transfer drive agent material infrared spectrum analysis
Fig. 1 is shown in using this method synthesis Micro Heterogeneous profile control agent (Micro Heterogeneous profile control agent 1) material infrared spectrogram.
It will be seen from figure 1 that 1659.81cm-1And 1452.86cm-1Neighbouring bands of a spectrum explanation-NH- exists, in 3190.52cm-1Place absorbs
Peak is the unsaturated hydrocarbon stretching vibration peak of phenyl ring, 2924.74cm-1Place is the absorption peak of-C-H, 1035.62cm-1With
1121.67cm-1Place is-SO3H characteristic absorption peak.Thus illustrate, α-methylstyrene (α-MSt) hydrophobic grouping phenyl ring and water-soluble
The heat and salinity tolerance group sulfonic acid group of property monomer 2- acrylamide-2-methylpro panesulfonic acid (AMPS) is in Micro Heterogeneous transfer drive
On agent material, show that copolyreaction successfully has occurred.
As shown in table 1, table 2, tested by 4 factor, 3 horizontal quadrature, obtain 9 groups of samples, choose wherein stability of emulsion compared with
Good 3 kinds, respectively Micro Heterogeneous profile control agent 1, Micro Heterogeneous profile control agent 2 and Micro Heterogeneous profile control agent 3 carries out subsequent
Experimental Characterization.
2, Micro Heterogeneous profile control agent partial size and particle diameter distribution and time relationship
(1) Micro Heterogeneous profile control agent partial size
During 3 hydration swelling of Micro Heterogeneous profile control agent 1, Micro Heterogeneous profile control agent 2 and Micro Heterogeneous profile control agent
Different moments Micro Heterogeneous profile control agent partial size test result (μm), which summarizes, is shown in Table 3.From table 3 it can be seen that microcosmic non-equal at 3 kinds
In matter profile control agent, 1 partial size of Micro Heterogeneous profile control agent is increased speed obvious quickening after aquation 72h, change of size amplitude after 240h
It is gradually reduced, 18 μm of ultimate size intermediate value, expansion multiple is more than 10, hence it is evident that be higher than other 2 Micro Heterogeneous profile control agent samples.
(2) Micro Heterogeneous profile control agent expansion multiple
Water-absorbent expanding multiple is the ratio between partial size and partial size before water swelling after the water swelling of Micro Heterogeneous profile control agent, reflection
Micro Heterogeneous profile control agent water swelling ability, value is bigger, and Micro Heterogeneous profile control agent water swelling ability is stronger, otherwise more
It is weak.
Expansion multiple calculation formula is
Q=(d2-d1)/d1 (1)
In formula, Q-expansion multiple, zero dimension；
d1And d2- for partial size after initial and expansion, μm.
Micro Heterogeneous profile control agent expansion multiple (median particle size) and time relationship are shown in Fig. 2.It can be seen that from shown in Fig. 2
Extend with hydration time, Micro Heterogeneous profile control agent partial size expansion multiple increases, and expansion rate is very fast before 72h, later expansion speed
Degree slows down.Compared with other Micro Heterogeneous profile control agents, " Micro Heterogeneous profile control agent 1 " partial size expansion rate starts after 72h
Accelerate, tends towards stability after 192h.From the aspect of aquation effect, that is, expansion multiple, 3 kinds of Micro Heterogeneous profile control agent performance superiority and inferiority
Relationship: " Micro Heterogeneous profile control agent 1 " is better than " Micro Heterogeneous profile control agent 2 " and " Micro Heterogeneous profile control agent 3 ".
3, Micro Heterogeneous profile control agent delays swollen effect in rock core
(1) Micro Heterogeneous profile control agent plugging effect
Delaying swollen closure in Micro Heterogeneous profile control agent rock core the results are shown in Table 4.From table 4, it can be seen that " Micro Heterogeneous transfer drive
1 " resistance coefficient of agent and residual resistance factor are greater than " Micro Heterogeneous profile control agent 2 " and " Micro Heterogeneous profile control agent 3 ".
(2) migration ability is transmitted
Micro Heterogeneous profile control agent 1 injects each section barometric gradient of rock core and time relationship is shown in Table 5.As can be seen from Table 5,
In Micro Heterogeneous profile control agent injection process, closer from injection end, barometric gradient is higher.Since Micro Heterogeneous profile control agent is infused
During entering there is " effect of end surface " in core entry end near zone, compared with other sections, entrance and " pressure tap 1 " section
Pressure gradient is higher.In the subsequent waterflooding stage, compared with other sections, entrance and " pressure tap 1 " section barometric gradient liter
High-amplitude is also larger, shows that the region Micro Heterogeneous profile control agent hold-up is larger.Barometric gradient is almost kept at " pressure tap 3 "
It is constant, show that Micro Heterogeneous profile control agent does not migrate to also herein.
The orthogonal test table of 1 microballoon Performance Influence Factor of table
2 orthogonal test specific formula of table composition
Table 3 different moments Micro Heterogeneous profile control agent partial size test result
Delay swollen closure result in 4 Micro Heterogeneous profile control agent rock core of table
5 Micro Heterogeneous profile control agent of table transmits migration ability
Not by the content being illustrated it is the prior art in the present embodiment, therefore is no longer repeated.
Micro Heterogeneous profile control agent prepared by the present invention has following excellent compared with existing Micro Heterogeneous profile control agent
Point: (1) expansion multiple increases by 80% or so (as shown in figure 3, wherein " Micro Heterogeneous profile control agent 1 " is synthesized using this method
Micro Heterogeneous profile control agent, " Micro Heterogeneous profile control agent 2 " and " Micro Heterogeneous profile control agent 3 " are on current oil field using more
Extensive two kinds of Micro Heterogeneous profile control agents, similarly hereinafter.) plugging effect can be improved；(2) speed of expansion slows down 10% or so (such as
Shown in Fig. 2), increase migration distance in Micro Heterogeneous profile control agent reservoir, improves Micro Heterogeneous profile control agent deep rock tunneling
Effect；(3) Micro Heterogeneous profile control agent delays swollen time and expansion multiple and is not influenced by solvent water salinity, heat and salt resistance compared with
It is good.
The above described is only a preferred embodiment of the present invention, be not intended to limit the present invention in any form, it is all
It is any simple modification, equivalent change and modification to the above embodiments according to the technical essence of the invention, still falls within
Technical solution of the present invention.
Claims (5)
1. a kind of Micro Heterogeneous profile control agent, which is characterized in that it is by heat and salinity tolerance monomer, major pharmaceutical, initiator, crosslinking
Agent, emulsifier, auxiliary agent, decentralized medium and water carry out polymerization reaction and form；Wherein the weight percent of heat and salinity tolerance monomer is 1
Weight percent to 5%, major pharmaceutical is 10 to 30%, the weight percent of initiator is 0.1 to 0.3%, the weight of crosslinking agent
Amount percentage be 0.05 to 0.1%, the weight percent of emulsifier is 10 to 12%, the weight percent of decentralized medium be 45 to
65%, the weight percent of auxiliary agent is 0.1 to 1%, remaining is water.
2. Micro Heterogeneous profile control agent according to claim 1, which is characterized in that
The heat and salinity tolerance monomer is 2- acrylamide-2-methylpro panesulfonic acid (AMPS)；
The major pharmaceutical is the mixture of acrylamide (AM), α-methylstyrene (α-MSt) and acrylic acid (AA), wherein third
The weight percent of acrylamide (AM) is 80 to 90%, and the weight percent of α-methylstyrene (α-MSt) is 5 to 7%, propylene
Sour (AA) is surplus；
The auxiliary agent is sodium hydroxide (NaOH)；
The initiator is ammonium persulfate (APS) and sodium sulfite (Na2SO3) mixture, wherein ammonium persulfate (APS), sulfurous
Sour sodium (Na2SO3) weight ratio be 2:1；
The crosslinking agent is N,N methylene bis acrylamide (MBA)；
The emulsifier is the mixture of tween (Tween) -80 and this disk (Span) -80, wherein the weight of Tween 80 and span 80
Amount ratio is 10:13；
The decentralized medium is atoleine；
The water is deionized water.
3. a kind of preparation method of Micro Heterogeneous profile control agent as described in claim 1, which is characterized in that including following step
It is rapid:
(1) match production of hybrid seeds liquid
Oily phase: atoleine is successively weighed according to formula rate, Tween-80 and Span-80, which are placed in small beaker, to stir evenly；
Water phase: a small beaker separately is taken, deionized water, heat and salinity tolerance monomer, major pharmaceutical, auxiliary agent are successively weighed according to formula rate
(NaOH) and crosslinking agent and being placed in beaker dissolves；
Initiator: a certain amount of deionized-distilled water is taken to dissolve a certain amount of ammonium persulfate (APS) and sodium sulfite (Na respectively2SO3) in
In two small beakers, sealed with preservative film spare；
Oily phase kind liquid is added in four-neck flask and is stirred, while water phase kind liquid is instilled dropwise in oily phase kind liquid, stirs pre-emulsification
It is started to warm up after 30min, until when certain temperature, the nitrogen charging gas shielded 30min into four-neck flask, while being instilled dropwise with needle tubing
Initiator is stated, 1h is reacted；
(2) dropping liquid is prepared
Oily phase: atoleine is successively weighed according to formula rate, Tween-80 and Span-80, which are placed in small beaker, to stir evenly；
Water phase: a small beaker separately is taken, deionized water, heat and salinity tolerance monomer, major pharmaceutical, auxiliary agent are successively weighed according to formula rate
(NaOH) and crosslinking agent and being placed in beaker dissolves；
Initiator: a certain amount of deionized-distilled water is taken to dissolve a certain amount of ammonium persulfate (APS) and sodium sulfite (Na respectively2SO3) in
In two small beakers, sealed with preservative film spare；
Oily phase dropping liquid is placed in a beaker stirring, while water phase dropping liquid is instilled dropwise in oily phase dropping liquid, stirs pre-emulsification
30min。
(3) polymerization reaction
After kind of liquid reacts 1 hour, the dropping liquid after pre-emulsification 30min is poured into constant pressure titration funnel, constant pressure is titrated into funnel
It is placed in four-neck flask, dropping liquid is instilled dropwise in the four-neck flask for filling kind of liquid, while nitrogen charging gas shielded 30min, and use needle
Pipe instills the initiator of dropping liquid in four-neck flask dropwise respectively.Then each neck mouth is blocked, reacts four hours, obtains into
Product.
4. the preparation method of Micro Heterogeneous profile control agent according to claim 3, which is characterized in that the heat and salinity tolerance list
The weight percent of body is 1 to 5%, the weight percent of major pharmaceutical is 10 to 30%, the weight percent of initiator be 0.1 to
0.3%, the weight percent of crosslinking agent is 0.05 to 0.1%, the weight percent of emulsifier is 10 to 12%, decentralized medium
Weight percent is 45 to 65%, the weight percent of auxiliary agent is 0.1 to 1%, remaining is deionized water.
5. the preparation method of Micro Heterogeneous profile control agent according to claim 3, which is characterized in that the heat and salinity tolerance list
Body is 2- acrylamide-2-methylpro panesulfonic acid (AMPS)；
The major pharmaceutical is acrylamide (AM), 2- acrylamide-2-methylpro panesulfonic acid (AMPS), α-methylstyrene (α-
MSt) and the mixture of acrylic acid (AA), wherein the weight percent of acrylamide (AM) is 80 to 90%, Alpha-Methyl benzene second
The weight percent of alkene (α-MSt) is 5 to 7%, and acrylic acid (AA) is surplus；
The auxiliary agent is sodium hydroxide (NaOH)；
The initiator is ammonium persulfate (APS) and sodium sulfite (Na2SO3) mixture, wherein ammonium persulfate (APS), sulfurous
Sour sodium (Na2SO3) weight ratio be 2:1；
The crosslinking agent is N,N methylene bis acrylamide (MBA)；
The emulsifier is the mixture of tween (Tween) -80 and this disk (Span) -80, wherein the weight of Tween 80 and span 80
Amount ratio is 10:13；
The decentralized medium is atoleine；
The water is deionized water.
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