CN109207137A - Polyacrylamide particle oil displacement agent and preparation method thereof - Google Patents
Polyacrylamide particle oil displacement agent and preparation method thereof Download PDFInfo
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- CN109207137A CN109207137A CN201710552256.7A CN201710552256A CN109207137A CN 109207137 A CN109207137 A CN 109207137A CN 201710552256 A CN201710552256 A CN 201710552256A CN 109207137 A CN109207137 A CN 109207137A
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/58—Compositions for enhanced recovery methods for obtaining hydrocarbons, i.e. for improving the mobility of the oil, e.g. displacing fluids
- C09K8/588—Compositions for enhanced recovery methods for obtaining hydrocarbons, i.e. for improving the mobility of the oil, e.g. displacing fluids characterised by the use of specific polymers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/52—Amides or imides
- C08F220/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
- C08F220/56—Acrylamide; Methacrylamide
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F4/00—Polymerisation catalysts
- C08F4/40—Redox systems
Abstract
The present invention relates to a kind of POLYACRYLAMIDE FLOODING agent and preparation method thereof.The polyacrylamide amine structure that there is the cross-linked network structure being centrally formed using polyfunctionality crosslinking agent as crosslinking and branching chain structure to coexist for POLYACRYLAMIDE FLOODING agent of the invention, wherein cross-linked structure ratio shared in entire polyacrylamide amine structure is 60~95%, and the polyfunctionality crosslinking agent is made by allyl glycidyl ether or (methyl) glycidyl acrylate and polyethylene polyamine reaction.Oil displacement agent of the invention while elasticity with higher, viscosity and deformation recovery capability, and can guarantee that there is excellent long-term anti-aging property in high temperature and high salt environment, be conducive to the application in tertiary oil recovery.
Description
Technical field
The present invention relates to polyacrylamide particle oil displacement agents and preparation method thereof, belong to the preparation and application of high molecular material
Field.
Background technique
Petroleum is the basic material of a kind of non-renewable resource and the energy and chemical industry, is had to the national economic development
Important function.But China's main oilfield has entered the middle and later periods of secondary recovery at present, the reservoir in oil field, oil reservoir situation are seriously bad
Change, often be high temperature and high salt type, only by tertiary oil recovery could about 60% residual petroleum it is effectively mined.This for
Guarantee that China's long-term energy safety and economic sustainable development have important practical significance.Polyacrylamide (PAM) has water-soluble
Property good and viscosity it is high the advantages that, for the crucial high molecular material of ideal tertiary oil recovery.But in practical applications, line style poly- third
Acrylamide oil displacement agent is easy to happen molecular chain rupture under shear action, also, PAM is water-soluble in the environment of underground high temperature and high salt
The solution viscosity and oil displacement efficiency of liquid are greatly reduced.
In tertiary oil recovery technology, fully crosslinked polyacrylamide is used usually as profile-controlling and plugging agent, because it is good
The swollen property of body to high permeability formation can carry out profile control processing adjust its permeability.But fully crosslinked polyacrylamide is due to crosslinking
Degree is high, and hardness is big, and morphotropism is poor, migrates difficult in hole, cannot play the role of oil displacement agent, therefore in tertiary oil recovery
Using being restricted.
Summary of the invention
The object of the present invention is to provide novel polyacrylamide particle oil displacement agents and preparation method thereof.
For this purpose, the present invention devises a kind of the advantages of combining linear polyacrylamide and full crosslinked polyacrylamide
The novel oil displacement agent being non-fully crosslinked, after which is injected into below stratum, due to the effect of pressure difference, the particle of gel
It is deformed through hole, drives remaining oil in hole mobile to producing well, reach preferable oil displacement efficiency.Drive of the invention
After finish effective solution conventional linear partially hydrolyzed polyacrylamide (PHPA) (HPAM) enters stratum, because dilution, degradation, absorption,
Acid-base property condition changes the problem of oil displacement agent rapid failure caused by various complicated reasons.
One aspect of the present invention provides a kind of POLYACRYLAMIDE FLOODING agent, have using polyfunctionality crosslinking agent as
It is crosslinked the polyacrylamide amine structure that the cross-linked network structure being centrally formed coexists with branching chain structure, wherein cross-linked structure is entire
Proportion is 60~95% in polyacrylamide amine structure, and the polyfunctionality crosslinking agent by allyl glycidyl ether or
(methyl) glycidyl acrylate and polyethylene polyamine reaction and be made.
Another aspect of the present invention provides a kind of method for preparing POLYACRYLAMIDE FLOODING agent, comprising the following steps:
(1) preparation of cross-linking agent solution: by molar ratio be 1: 2~5 polyethylene polyamine and allyl glycidyl ether or
(methyl) glycidyl acrylate is soluble in water, so that the mass fraction of solute is 3-10%, it is then anti-at 50~85 DEG C
It answers, obtains polyfunctional crosslinking agent's solution；
(2) acrylamide polymerization reacts: being made aqueous solution for 100 parts of acrylamides are soluble in water, has been added 0.5~5 part
Cross-linking agent solution obtained；It is 8~10 that 0.002~0.04 part of organic amine, which is added, and adjusts solution ph；By gained reactant plus
Enter in adiabatic reaction kettle, be passed through inert gas deoxygenation, 0.03~0.05 part of persulfate is added at 5~30 DEG C of temperature and causes instead
It answers, carries out adiabatic polymerisation reaction under inert gas protection, after system gel, continuation is reacted 1~4 hour at 50-90 DEG C,
Obtain the block-like POLYACRYLAMIDE FLOODING agent product of glue.
It is characteristic of the invention that using polyethylene polyamine and allyl glycidyl ether or (methyl) glycidyl
The polyfunctional crosslinking agent of Lipase absobed is as crosslinking center, and using persulfate as oxidant, organic amine is reducing agent and promotor structure
At redox initiation system, the polyacrylamide particle oil displacement agent with polyfunctionality crosslinking center is prepared.The oil displacement agent is same
When elastic (elasticity modulus is up to 30Pa) with higher, sticky (viscosity is up to 20mPas) and deformation recovery capability, and
It can guarantee that there is excellent long-term anti-aging property in high temperature and high salt environment, be more advantageous to answering in tertiary oil recovery
With.
Detailed description of the invention
Fig. 1 is the nucleus magnetic hydrogen spectrum figure of allyl glycidyl ether and its crosslinking agent that preparation is reacted with tetraethylenepentamine.
It will be seen from figure 1 that on allyl glycidyl ether molecule with two chemical environment differences on ehter bond adjacent carbons
Hydrogen atom become identical two hydrogen of chemical environment and mobile to low field direction after reacting with tetraethylenepentamine；Epoxy group
Carbon on the different hydrogen of two chemical environments after being reacted with tetraethylenepentamine chemical environment reach unanimity；Meanwhile allyl
Vinyl on glycidol ether is rear and unchanged before the reaction, illustrates that the reaction is completed on the basis of retaining vinyl double bond
The opening of epoxy group.
Fig. 2 is the liquid chromatograph mass spectrography test result of crosslinking agent shown in Fig. 1.
Figure it is seen that molecular weight is 303,417,531, i.e., 1,2,3 allyl contracting of access in tetraethylenepentamine
There is apparent peak in the component of water glycerin ether, illustrates that crosslinking agent is a kind of mixture, wherein tetraethylenepentamine and two and three
The polyfunctional compound that a allyl glycidyl ether is reacted and formed is main product.
Fig. 3 is that the deal pair of different cross-linking agent solutions is added in the identical situation of embodiment 1,10,11 in other conditions
The storage modulus change curve for the suspension that polymeric articles are formed in salt water；
Fig. 4 is that the deal pair of different cross-linking agent solutions is added in the identical situation of embodiment 1,10,11 in other conditions
The viscosity change curve graph for the suspension that polymeric articles are formed in salt water；
Fig. 5 is that the polyacrylamide particle oil displacement agent that the prepares modulus in ageing process becomes with ageing time in embodiment 10
The curve graph of change；
Fig. 6 is that the polyacrylamide particle oil displacement agent prepared in embodiment 10 becomes in ageing process medium viscosity with ageing time
The curve graph of change；
Using the polyacrylamide gel oil displacement agent of novel long-chain polyfunctional crosslinking agent preparation it can be seen from Fig. 5, Fig. 6
In ageing process, suspension is able to maintain stabilization within considerable time, this explanation is by novel more officials produced by the present invention
The polyacrylamide gel oil displacement agent of energy crosslinking agent preparation has stable cross-linked network structure, remains under high temperature and high salt environment
Inhibit the destruction of network structure, there is excellent ageing-resistant performance.Simultaneously with the extension of ageing time, the viscosity of the oil displacement agent
Lasting to rise, in ageing process, partial cross-linked network fracture increases branched chain, has achieved the effect that increasing stick this explanation.
Fig. 7 is the online rheometer test figure of the polyacrylamide gel prepared in embodiment 10
As shown in fig. 7, the storage modulus G' and Loss modulus G " of polyacrylamide gel are gradually with the progress of reaction
Reach a higher value, fissipation factor tan δ may finally be maintained at 0.1 or so.Its cross-linked network being formed in situ ensure that
The high modulus of polyacrylamide gel particle and the deformation recovery capability in migration process, and when gel particle is between rock core
When gap migration is by extruding is pulled, polyacrylamide gel particle can dissipate to external energy by the sliding of branched chain,
And then a possibility that substantially reducing brittle fracture, to assign the gel energy dissipation capability excellent in deformation process.
Fig. 8 is the frequency scanning test chart of the polyacrylamide gel prepared in embodiment 10
Fig. 9 is the strain sweep test chart of the polyacrylamide gel prepared in embodiment 10
From figure 8, it is seen that the storage modulus G ' and Loss modulus G " of gel occur with the quickening of vibration frequency
It is apparent to rise.Under high frequency state, there is apparent increase in the storage modulus of network.This phenomenon explanation, in the gel
Network structure in not be entirely covalently cross-linked network structure, there are still a certain amount of branched chains.In addition, can from Fig. 9
To find out, with the increase of strain, the storage modulus G ' of gel is decreased obviously.This is just because of the branching in gel network
Caused by the sliding of chain.Just because of the presence of these branched chains, it ensure that gel exists pair when being squeezed, rubbing by external force
The loss of external force avoids brittle fracture in turn, improves its toughness.
Figure 10 is single tube rock core seepage apparatus schematic diagram, in which:
1, oil pump；2, saline solution；3, oil displacement agent suspension；4, magnetic stirring apparatus；5, pressure gauge；6, sand-filling tube model；
Figure 11 is two-tube rock core seepage apparatus schematic diagram, in which:
1, pressure gauge；2, sand-filling tube model；
Figure 12 is that fill out sand tube pressure at two ends is outstanding with the polyacrylamide particle prepared in embodiment 10 in rock core Seepage Experiment
The change curve of supernatant liquid injected slurry volume.Experiment uses homemade sand-filling tube model, and fill out sand tube permeability is 1500 × 10-3μm2,
The salt water that water is salinity 19334mg/L is injected, fluid injection rate is 0.5m L/min, and experimental temperature is 70 DEG C.
As seen from Figure 12, in the water drive stage, pressure change is smaller, quickly reaches equilibrium state；When using novel length
After the polyacrylamide particle oil displacement agent of chain polyfunctional crosslinking agent preparation carries out displacement, pressure increases sharply, and shows plugging action
Formation, the permeability reduction of fill out sand tube；After pressure reaches maximum value, pressure is fluctuated, until balance.Pressure curve wave
It is dynamic to show polyacrylamide particle prepared by the present invention in porous media after " a particle accumulation-particles compress-
Grain deformation passes through " migration process, when particle block speed it is equal with the speed that particle deformation passes through when, pressure be reach flat
Weighing apparatus, fluid also approach equilibrium state to the adjustment of fill out sand tube permeability.After subsequent waterflooding starts, partial particulate is rushed to open, fill out sand tube
Permeability increases, and pressure is begun to decline, but remains to reach 2MPa or so when final balance.Single tube rock core Seepage Experiment shows this hair
The polymer oil-displacing agent of bright preparation has excellent profile modification simultaneously in rock core.
Figure 13 is the two-tube parallel split-flow amount experimental result picture of the polyacrylamide particle prepared in embodiment 10.Experiment is adopted
It is respectively 5000 × 10 with permeability-3um2With 1000 × 10-3um2Two parallel fill out sand tube studied.
As can be seen from Figure 13, the fill out sand tube of 5000mD is blocked gradually after poly- drive, while in 1000mD fill out sand tube
Liquid proportional is flowed out to increase.After subsequent waterflooding, there is no inverting, the outflow liquid proportional of 1000mD still exists the outflow ratio of the two
Increase.This phenomenon explanation, macrovoid is blocked by particle in simulation core during poly- drive, realizes fluid diversion.And water
Polymer beads remain in macrovoid after drive, and the water not injected is washed open.Illustrate polymer flooding prepared by the present invention
Finish has efficient section corrective action in oil reservoir.
Specific embodiment
An embodiment according to the present invention, the formula for synthesizing polyacrylamide gel oil displacement agent are as follows:
And in following processing steps and technological parameter preparation:
A. molar ratio is sweet for 1: 2~5 polyethylene polyamine and allyl glycidyl ether or (methyl) acrylic acid shrink
Grease is soluble in water, and the mass fraction of solute is 3~10%, reacts at 50~85 DEG C, obtains polyfunctional crosslinking agent's solution；
B. aqueous solution is made 100 parts of acrylamides are soluble in water and 0.5~5 part of cross-linking agent solution obtained is added；
It is 8~10 that 0.002~0.04 part of organic amine, which is added, and adjusts solution ph；Gained reactant is added in adiabatic reaction kettle and is led to
Enter inert gas deoxygenation, 0.03~0.05 part of persulfate initiation reaction is added at 5~30 DEG C of temperature, in inert gas shielding
Lower progress adiabatic polymerisation reaction, after system gel, continuation is reacted 1~4 hour at 50-90 DEG C, obtains glue block-like poly- third
Acrylamide oil displacement agent product.
Above-mentioned steps a is the preparation step of cross-linking agent solution.Polyethylene polyamine therein includes containing 2~4 ethylidene
With the amine substance of 2~5 primary amine or secondary amine group, preferably have longer chain structure simultaneous with multiple primary amine or secondary amine group
The amine substance of (at least one primary amine, preferably entirely primary amine), for example, tetraethylenepentamine, triethylene tetramine, divinyl three
Amine etc..
Polyethylene polyamine and allyl glycidyl ether or (methyl) glycidyl acrylate reacting in aqueous solution
For opening.By taking the reacting of allyl glycidyl ether and tetraethylenepentamine as an example, such as it will be seen from figure 1 that allyl
It is reacted from two different hydrogen atoms of chemical environment on ehter bond adjacent carbons with tetraethylenepentamine on base glycidol ether molecule
After become identical two hydrogen of chemical environment and mobile to low field direction；Two chemical environments on the carbon of epoxy group are different
Hydrogen chemical environment after reacting with tetraethylenepentamine reaches unanimity；Meanwhile the vinyl on allyl glycidyl ether is reacting
Front and back is simultaneously unchanged, illustrates that the reaction completes the opening of epoxy group on the basis of retaining vinyl double bond.
The reaction product of polyethylene polyamine and allyl glycidyl ether or (methyl) glycidyl acrylate is a kind of
Mixture mainly shrinks comprising polyethylene polyamine and one, two and three allyl glycidyl ether or (methyl) acrylic acid
The addition reaction product of glyceride.Such as figure it is seen that molecular weight is 303,417,531, i.e., accessed in tetraethylenepentamine
1, there is apparent peak in the component of 2,3 allyl glycidyl ethers.
In the preparation of above-mentioned polyfunctionality crosslinking agent, the yield of reaction product is related to reaction temperature and reaction time.Temperature
Degree is high, the addition product of time long available height ratio, on the contrary then will form low-ratio product.Under certain reaction condition,
It can get crosslinker product of the average vinyl content in 1~3 (molar ratio) range.In general, reaction temperature is 50~85
DEG C, preferably 55~80 DEG C, more preferable 60~80 DEG C.Reaction time general control is 5~7 hours.
Step b is acrylamide polymerization reaction step.It wherein, is to hand over the polyfunctional crosslinking agent prepared in above-mentioned steps a
Connection center, in the presence of redox initiation system (wherein persulfate is oxidant, and organic amine is reducing agent and promotor),
In an aqueous medium, the polymerization reaction for carrying out acrylamide under inert gas protection, obtains POLYACRYLAMIDE FLOODING agent gel.
Organic amine in step b includes that aliphatic diamine, aliphatic tertiary amine or their mixture etc. have relatively by force
The organic amine of reproducibility, plays the role of reducing agent and promotor in the reaction system.The example of organic amine may include tetramethyl
Base ethylenediamine, pentamethyl-diethylenetriamine etc..
Persulfate includes potassium peroxydisulfate, sodium peroxydisulfate etc..
Inert gas includes nitrogen etc..It is passed through nitrogen etc. and does not require nothing more than the oxygen removed in reactor, also have stirring concurrently and make
With, therefore all need to be passed through nitrogen before reaction system starts polymerization.It is passed through the degree of nitrogen discharge oxygen, also influences persulfuric acid
The efficiency of initiation of salt.
Since reacting for polyacrylamide and polyfunctional crosslinking agent is one and is cross-linked in situ reaction, so reaction temperature, coagulates
There is conclusive influence in the glue time on the structure of polyacrylamide.In the above-mentioned multifunctional cross-linking system polyacrylamide of the present invention
In the preparation method of grain oil displacement agent, the temperature of initiated polymerization is lower, and reaction progress speed is slower, and crosslinking degree is high；Temperature
Too high, reaction carries out too fast, and crosslinking degree is low, and suitable initiation temperature is 5~30 DEG C, preferably 8~18 DEG C.In addition.Polymerization
Reaction carries out in thermal insulation system, there is no heat exchange with the external world.In general, being 50~90 in reaction temperature after gel
The reaction was continued at DEG C, such as is maintained at 75~85 DEG C the reaction was continued, until obtaining the block-like POLYACRYLAMIDE FLOODING agent product of glue.
Reaction time after gel is generally 1~4 hour, preferably 2~4 hours.
The preparation method of multifunctional cross-linking system polyacrylamide particle oil displacement agent of the invention can also include that will be made
Gluey oil displacement agent product the post-processing such as shredded, dried, being crushed, being sieved, to obtain particle or powdery oil displacement agent.
A specific embodiment according to the present invention, acrylamide polymerization reaction step specifically include: by 100 parts of propylene
Amide, which is dissolved in 150~180 parts of deionized water, to be made aqueous solution and 0.5~5 part of cross-linking agent solution obtained is added.It is added
0.002~0.04 part of organic amine and to adjust solution ph be 8~10, uniformly mixed reactant is added in adiabatic reaction kettle simultaneously
It is passed through inert gas deoxygenation, 0.03~0.05 part of persulfate initiation reaction is added at 5~30 DEG C of temperature, to system gel
Afterwards, continue to react 2~4 hours at 50-90 DEG C, product stripping and slicing is shredded into drying, crushing, screening, obtains particle oil displacement agent.
The multifunctional cross-linking system POLYACRYLAMIDE FLOODING agent of above method preparation through the invention is a kind of incomplete
The POLYACRYLAMIDE FLOODING agent of crosslinking, have using polyfunctionality crosslinking agent as the cross-linked network structure that is centrally formed of crosslinking and
The polyacrylamide amine structure that branched chain coexists, wherein cross-linked structure in entire polyacrylamide amine structure proportion be 60~
95%, such as 60~70%, 70~80%, 70~75%, 80~90% etc..
Cross-linked structure proportion in entire polyacrylamide amine structure can measure in accordance with the following methods: weigh just prothyl
Amount is the powdery oil displacement agent (generally about 0.5g) of M1, after being sufficiently swollen (generally seven days) in water (about 200ml) at room temperature, mistake
Filtering resulting gel particle is its crosslinking moieties, and being baked to weighing quality is M2, and (M2/M1*100%) is its crosslinking
Ratio of the structure in entire polyacrylamide amine structure.
In the present invention, due to using the polyfunctional crosslinking agent with longer chain as crosslinking center, and acrylamide is controlled
Polymerization reaction carries out at a lower temperature, and polyfunctional crosslinking agent's molecule is uniformly distributed in the polymer, forms comparatively perfect
Cross-linked network structure with high cross-link intensity remains to the destruction for inhibiting network structure under high temperature and high salt environment, has excellent
Ageing-resistant performance.Moreover, because imparting the excellent tensile property of polymer and stress dissipativeness there are branching chain structure
Can, it ensure that gel avoids brittle fracture in turn in the presence of the loss to external force when being squeezed, rubbing by external force, improve tough
Property.
Polyfunctional crosslinking agent of the invention and the POLYACRYLAMIDE FLOODING agent prepared by the crosslinking agent are with excellent heatproof
Salt resistance and anti-shear performance can satisfy the rigors of subsurface deposit environment, the aging in 85 DEG C, 30000 salinity salt water
90 days, still it is able to maintain 70% modulus.In addition, polyfunctional crosslinking agent of the invention and the polyacrylamide prepared by the crosslinking agent
Oil displacement agent can play the role of good profile control displacement in rock core, and two-tube rock core Seepage Experiment shows it with efficient section
Corrective action.
The present invention is specifically described below by embodiment, it is necessary to which indicated herein is that the present embodiment is served only for pair
The present invention is further described, and should not be understood as limiting the scope of the invention, and the person skilled in the art in the field can
Some nonessential modifications and adaptations are made with the content according to aforementioned present invention.
Following correlated performance test has been carried out as follows to polymer oil-displacing agent sample made from following embodiment:
1. rheology testing
Rheology testing is carried out using the AR2000 EX type torque rheometer of TA company.Test is swept including dynamic frequency
It retouches to scan with speed of steady state and test, all tests are carried out at 25 DEG C, sample concentration 800mg/L, salinity
30000mg/L(Ca2+,Mg2+≥2000mg/L).Dynamic frequency test carries out under single-frequency, selected frequency f=1Hz, stress τ
The average value of lower 5 test results of=0.1Pa is the modulus G ' of solution.Speed of steady state sweep test is selected under single shear rate
Time sweep equally takes the average value of 5 tests for the viscosity of solution, shear rate v=7.34s-1.Test the salt water that uses for
According to the simulation water that Shengli Oil Field difference oil reservoir salinity and salt ionic concentration are prepared, different saline formulations are as shown in table 1.
The different salinity saline formulation tables of table 1
| Salinity | H2O | NaCl | CaCl2 | MgCl2·6H2O | Na2SO |
| 6666mg/L | 1000mL | 6.191g | 0.2414g | 0.3514g | 0.0696g |
| 19334mg/L | 1000mL | 17.4578g | 1.1433g | 0.863g | 0 |
| 30000mg/L | 1000mL | 27.3067g | 1.11g | 3.833g | 0 |
| 50000mg/L | 1000mL | 42.758g | 2.825g | 8.917g | 0 |
2. ageing properties are tested
Test concentration be 800mg/L sample under anaerobic, salinity 30000mg/L (Ca at 85 DEG C2+, Mg2+
>=2000mg/L) solution in long-term ageing-resistant performance, and determine body phase of the sample after long-term ageing with torque rheometer
Viscosity.
3. single tube rock core Seepage Experiment
Experiment porous media used is self-control fill out sand tube, and the permeability of a length of 30cm, internal diameter 2.5cm, fill out sand tube are
(1500±15)×10-3um2, pore volume (pore volume) is 50 ± 0.5cm3.Entire Seepage Experiment is in digital temperature-controlled box
Middle progress, fluid injection rate are 0.5mL/min, and experimental temperature is 70 DEG C.
Experimental method: first into fill out sand tube inject salinity be 19334mg/L salt water, record at regular intervals into
Mouth pressure.After pressure balance, change the polymer oil-displacing agent suspension of note 2000mg/L, time recording pressure, to pressure balance
Subsequent waterflooding is carried out afterwards to balance.
4. two-tube rock core Seepage Experiment
Test is respectively (1000 ± 10) × 10 using the permeability of high permeability and low-permeability fill out sand tube-3μm2With
(5000±15)×10-3μm2, the total pore size volume of two parallel seepage flow pipes is 101.6 ± 0.5cm3.It is infused in a manner of closing note point and adopting
Enter salt water and polymer oil-displacing agent suspension, injection rate 0.5mL/min, experimental temperature is 70 DEG C.
Experimental method: after injecting 1PV (pore volume) salinity is 19334mg/L salt water, change note 2PV 2000mg/L
Polymer oil-displacing agent suspension, carry out subsequent waterflooding later.Time recording pressure change and high and low permeability in experimentation
The Liquid output of fill out sand tube, by analysis fractional flow curves come the transfer drive performance of comparative study polymer oil-displacing agent suspension.
In following embodiment, involved component number, percentage are mass parts in addition to special instruction
Number, percentage.
The synthesis of crosslinking agent:
Embodiment A: tetraethylenepentamine and allyl glycidyl ether that molar ratio is 1:4 are dissolved in 100 parts of water, adjusted
The mass fraction of solute is 6.54%, and prepared reactant is filled in the reaction equipped with condenser, temperature controller and blender
In setting, is reacted 6 hours at 75 DEG C, polyfunctional crosslinking agent's solution A is prepared.
Reactant allyl glycidyl ether and the nuclear magnetic resonance spectroscopy of reaction product are as shown in Figure 1, gained crosslinking agent
Liquid chromatograph mass spectrography test results are shown in figure 2.AV600 model nuclear-magnetism of the nuclear magnetic resonance spectroscopy in Bruker company
It is carried out on resonance instrument, liquid chromatography-mass spectrography carries out in the chromatography unit of the 1100MSD model of Aqilent company, chromatostrip
Part are as follows: use reverse phase silica gel column, mobile phase is methanol, flow velocity 1.5ml/min.Mass Spectrometry Conditions are as follows: the source EI, ion source temperature are
200 DEG C, electron energy 70eV.
Embodiment B: the tetraethylenepentamine that molar ratio is 1: 4 is dissolved in 100 parts of water with allyl glycidyl ether, is adjusted
The mass fraction of solute is 6.54%, and prepared reactant is filled in the reaction equipped with condenser, temperature controller and blender
In setting, is reacted 6 hours at 50 DEG C, polyfunctional crosslinking agent's solution B is prepared
Embodiment C: the tetraethylenepentamine that molar ratio is 1: 4 is dissolved in 100 parts of water with allyl glycidyl ether, is adjusted
The mass fraction of solute is 6.54%, and prepared reactant is filled in the reaction equipped with condenser, temperature controller and blender
In setting, is reacted 6 hours at 60 DEG C, polyfunctional crosslinking agent's solution C is prepared.
Embodiment D: the tetraethylenepentamine that molar ratio is 1: 4 is dissolved in 100 parts of water with allyl glycidyl ether, is adjusted
The mass fraction of solute is 6.54%, and prepared reactant is filled in the reaction equipped with condenser, temperature controller and blender
In setting, is reacted 6 hours at 80 DEG C, polyfunctional crosslinking agent's solution D is prepared.
Embodiment E: the tetraethylenepentamine that molar ratio is 1: 4 is dissolved in 100 parts of water with allyl glycidyl ether, is adjusted
The mass fraction of solute is 6.54%, and prepared reactant is filled in the reaction equipped with condenser, temperature controller and blender
In setting, is reacted 5 hours at 75 DEG C, polyfunctional crosslinking agent's solution E is prepared.
Embodiment F: the tetraethylenepentamine that molar ratio is 1: 4 is dissolved in 100 parts of water with allyl glycidyl ether, is adjusted
The mass fraction of solute is 6.54%, and prepared reactant is filled in the reaction equipped with condenser, temperature controller and blender
In setting, is reacted 7 hours at 75 DEG C, polyfunctional crosslinking agent's solution F is prepared.
Embodiment G: the tetraethylenepentamine that molar ratio is 1: 4 is dissolved in 100 parts of water with glycidyl methacrylate,
The mass fraction for adjusting solute is 6.54%, by prepared reactant equipped with the anti-of condenser, temperature controller and blender
It answers in device, is reacted 6 hours at 75 DEG C, polyfunctional crosslinking agent's solution G is prepared.
Embodiment H: the triethylene tetramine that molar ratio is 1: 4 is dissolved in 100 parts of water with allyl glycidyl ether, is adjusted
The mass fraction of solute is 6.54%, and prepared reactant is filled in the reaction equipped with condenser, temperature controller and blender
In setting, is reacted 6 hours at 75 DEG C, polyfunctional crosslinking agent's Solution H is prepared.
Embodiment I: the tetraethylenepentamine that molar ratio is 1: 2 is dissolved in 100 parts of water with allyl glycidyl ether, is adjusted
The mass fraction of solute is 6.54%, and prepared reactant is filled in the reaction equipped with condenser, temperature controller and blender
In setting, is reacted 6 hours at 75 DEG C, polyfunctional crosslinking agent's solution I is prepared.
Embodiment J: the tetraethylenepentamine that molar ratio is 1: 5 is dissolved in 100 parts of water with allyl glycidyl ether, is adjusted
The mass fraction of solute is 6.54%, and prepared reactant is filled in the reaction equipped with condenser, temperature controller and blender
In setting, is reacted 6 hours at 75 DEG C, polyfunctional crosslinking agent's solution J is prepared.
Embodiment K: the tetraethylenepentamine that molar ratio is 1: 4 is dissolved in 100 parts of water with glycidyl acrylate, is adjusted
The mass fraction of solute is 6.54%, and prepared reactant is filled in the reaction equipped with condenser, temperature controller and blender
In setting, is reacted 6 hours at 75 DEG C, polyfunctional crosslinking agent's solution G is prepared.
The preparation of multifunctional cross-linking system polyacrylamide gel:
Embodiment 1
100 parts of acrylamides are dissolved in 150 parts of deionized water, aqueous solution is made and 1 part of crosslinking agent obtained is added
Solution A.It is 9 that 0.002 part of tetramethylethylenediamine, which is added, and adjusts solution pH value, is injected in adiabatic reaction kettle, at 12 DEG C of temperature,
After letting nitrogen in and deoxidizing 15 minutes, 0.03 part of potassium peroxydisulfate initiation reaction of 50 parts of water dissolution is added, carries out adiabatic polymerisation, it is solidifying to system
After glue, continuation is reacted 2 hours at 85 DEG C, by product chopping drying, is crushed, screening, is obtained particle oil displacement agent.
Performance test: the elastic modulus G ' measured under its 200 μm of spacing of particle oil displacement agent made from embodiment 1=
7.998Pa；Viscosities il=the 13.25mPa.s measured under 1000 μm of spacing.
Embodiment 2
100 parts of acrylamides are dissolved in 150 parts of deionized water, aqueous solution is made and 1 part of crosslinking agent obtained is added
B solution.It is 9 that 0.002 part of tetramethylethylenediamine, which is added, and adjusts solution pH value, is injected in adiabatic reaction kettle, at 12 DEG C of temperature,
After letting nitrogen in and deoxidizing 15 minutes, 0.03 part of potassium peroxydisulfate initiation reaction of 50 parts of water dissolution is added, carries out adiabatic polymerisation, it is solidifying to system
After glue, continuation is reacted 2 hours at 85 DEG C, by product chopping drying, is crushed, screening, is obtained particle oil displacement agent.
Performance test: the elastic modulus G ' measured under its 200 μm of spacing of particle oil displacement agent made from embodiment 2=
5.378Pa；Viscosities il=the 15.09mPa.s measured under 1000 μm of spacing.
Embodiment 3
100 parts of acrylamides are dissolved in 150 parts of deionized water, aqueous solution is made and 1 part of crosslinking agent obtained is added
C solution.It is 9 that 0.002 part of tetramethylethylenediamine, which is added, and adjusts solution pH value, is injected in adiabatic reaction kettle, at 12 DEG C of temperature,
After letting nitrogen in and deoxidizing 15 minutes, 0.03 part of potassium peroxydisulfate initiation reaction of 50 parts of water dissolution is added, carries out adiabatic polymerisation, it is solidifying to system
After glue, continuation keeps the temperature 2 hours at 85 DEG C, by product chopping drying, crushes, screening, obtains particle oil displacement agent.
Performance test: the elastic modulus G ' measured under its 200 μm of spacing of particle oil displacement agent made from embodiment 3=
6.282Pa；Viscosities il=the 14.77mPa.s measured under 1000 μm of spacing.
Embodiment 4
100 parts of acrylamides are dissolved in 150 parts of deionized water, aqueous solution is made and 1 part of crosslinking agent obtained is added
Solution D.It is 9 that 0.002 part of tetramethylethylenediamine, which is added, and adjusts solution pH value, is injected in adiabatic reaction kettle, at 12 DEG C of temperature,
After letting nitrogen in and deoxidizing 15 minutes, 0.03 part of potassium peroxydisulfate initiation reaction of 50 parts of water dissolution is added, carries out adiabatic polymerisation, it is solidifying to system
After glue, continuation is reacted 2 hours at 85 DEG C, by product chopping drying, is crushed, screening, is obtained particle oil displacement agent.
Performance test: the elastic modulus G ' measured under its 200 μm of spacing of particle oil displacement agent made from embodiment 4=
8.486Pa；Viscosities il=the 12.20mPa.s measured under 1000 μm of spacing.
Embodiment 5
100 parts of acrylamides are dissolved in 150 parts of deionized water, aqueous solution is made and 1 part of crosslinking agent obtained is added
E solution.It is 9 that 0.002 part of tetramethylethylenediamine, which is added, and adjusts solution pH value, is injected in adiabatic reaction kettle, at 12 DEG C of temperature,
After letting nitrogen in and deoxidizing 15 minutes, 0.03 part of potassium peroxydisulfate initiation reaction of 50 parts of water dissolution is added, carries out adiabatic polymerisation, it is solidifying to system
After glue, continuation is reacted 2 hours at 85 DEG C, by product chopping drying, is crushed, screening, is obtained particle oil displacement agent.
Performance test: the elastic modulus G ' measured under its 200 μm of spacing of particle oil displacement agent made from embodiment 5=
6.054Pa；Viscosities il=the 14.30mPa.s measured under 1000 μm of spacing.
Embodiment 6
100 parts of acrylamides are dissolved in 150 parts of deionized water, aqueous solution is made and 1 part of crosslinking agent obtained is added
F solution.It is 9 that 0.002 part of tetramethylethylenediamine, which is added, and adjusts solution pH value, is injected in adiabatic reaction kettle, at 12 DEG C of temperature,
After letting nitrogen in and deoxidizing 15 minutes, 0.03 part of potassium peroxydisulfate initiation reaction of 50 parts of water dissolution is added, carries out adiabatic polymerisation, it is solidifying to system
After glue, continuation is reacted 2 hours at 85 DEG C, by product chopping drying, is crushed, screening, is obtained particle oil displacement agent.
Performance test: the elastic modulus G ' measured under its 200 μm of spacing of particle oil displacement agent made from embodiment 6=
8.283Pa；Viscosities il=the 11.50mPa.s measured under 1000 μm of spacing.
Embodiment 7
100 parts of acrylamides are dissolved in 150 parts of deionized water, aqueous solution is made and 1 part of crosslinking agent obtained is added
G solution.It is 9 that 0.002 part of tetramethylethylenediamine, which is added, and adjusts solution pH value, is injected in adiabatic reaction kettle, at 12 DEG C of temperature,
After letting nitrogen in and deoxidizing 15 minutes, 0.03 part of potassium peroxydisulfate initiation reaction of 50 parts of water dissolution is added, carries out adiabatic polymerisation, it is solidifying to system
After glue, continuation is reacted 2 hours at 85 DEG C, by product chopping drying, is crushed, screening, is obtained particle oil displacement agent.
Performance test: the elastic modulus G ' measured under its 200 μm of spacing of particle oil displacement agent made from embodiment 7=
7.386Pa；Viscosities il=the 12.85mPa.s measured under 1000 μm of spacing.
Embodiment 8
100 parts of acrylamides are dissolved in 150 parts of deionized water, aqueous solution is made and 1 part of crosslinking agent obtained is added
Solution A.0.02 part of pentamethyl-diethylenetriamine, 0.002 part of tetramethylethylenediamine is added and to adjust solution pH value be 9, injection is exhausted
In thermal response kettle, at 12 DEG C of temperature, after letting nitrogen in and deoxidizing 15 minutes, 0.03 part of potassium peroxydisulfate that the dissolution of 50 parts of water is added causes instead
It answers, carries out adiabatic polymerisation, after system gel, continue to react at 85 DEG C temperature 2 hours, by product chopping drying, crush, sieve
Point, obtain particle oil displacement agent.
Performance test: the elastic modulus G ' measured under its 200 μm of spacing of particle oil displacement agent made from embodiment 8=
6.255Pa；Viscosities il=the 13.01mPa.s measured under 1000 μm of spacing.
Embodiment 9
100 parts of acrylamides are dissolved in 150 parts of deionized water, aqueous solution is made and 1 part of crosslinking agent obtained is added
Solution A.It is 9 that 0.04 part of pentamethyl-diethylenetriamine, which is added, and adjusts solution pH value, is injected in adiabatic reaction kettle, in 12 DEG C of temperature
Under, after letting nitrogen in and deoxidizing 15 minutes, 0.03 part of potassium peroxydisulfate initiation reaction of 50 parts of water dissolution is added, adiabatic polymerisation is carried out, to body
It is after gel, continuation is reacted 2 hours at 85 DEG C, by product chopping drying, is crushed, screening, is obtained particle oil displacement agent.
Performance test: the elastic modulus G ' measured under its 200 μm of spacing of particle oil displacement agent made from embodiment 9=
7.291Pa；Viscosities il=the 14.11mPa.s measured under 1000 μm of spacing.
Embodiment 10
100 parts of acrylamides are dissolved in 150 parts of deionized water, aqueous solution is made and 3 parts of crosslinking agents obtained are added
Solution A.It is 9 that 0.002 part of tetramethylethylenediamine, which is added, and adjusts solution pH value, is injected in adiabatic reaction kettle, at 12 DEG C of temperature,
After letting nitrogen in and deoxidizing 15 minutes, 0.03 part of potassium peroxydisulfate initiation reaction of 50 parts of water dissolution is added, carries out adiabatic polymerisation, it is solidifying to system
After glue, continuation is reacted 2 hours at 85 DEG C, by product chopping drying, is crushed, screening, is obtained particle oil displacement agent.
Performance test: the elastic modulus G ' measured under its 200 μm of spacing of particle oil displacement agent made from embodiment 10=
22.52Pa；Viscosities il=the 2.344mPa.s measured under 1000 μm of spacing.
Embodiment 11
100 parts of acrylamides are dissolved in 150 parts of deionized water, aqueous solution is made and 5 parts of crosslinking agents obtained are added
Solution A.It is 9 that 0.002 part of tetramethylethylenediamine, which is added, and adjusts solution pH value, is injected in adiabatic reaction kettle, at 12 DEG C of temperature,
After letting nitrogen in and deoxidizing 15 minutes, 0.03 part of potassium peroxydisulfate initiation reaction of 50 parts of water dissolution is added, carries out adiabatic polymerisation, it is solidifying to system
After glue, continuation is reacted 2 hours at 85 DEG C, by product chopping drying, is crushed, screening, is obtained particle oil displacement agent.
Performance test: the elastic modulus G ' measured under its 200 μm of spacing of particle oil displacement agent made from embodiment 11=
28.46Pa；Viscosities il=the 2.011mPa.s measured under 1000 μm of spacing.
Embodiment 12
100 parts of acrylamides are dissolved in 150 parts of deionized water, aqueous solution is made and 1 part of crosslinking agent obtained is added
Solution A.It is 9 that 0.002 part of tetramethylethylenediamine, which is added, and adjusts solution pH value, is injected in adiabatic reaction kettle, at 12 DEG C of temperature,
After letting nitrogen in and deoxidizing 15 minutes, 0.04 part of potassium peroxydisulfate initiation reaction of 50 parts of water dissolution is added, carries out adiabatic polymerisation, it is solidifying to system
After glue, continuation is reacted 2 hours at 85 DEG C, by product chopping drying, is crushed, screening, is obtained particle oil displacement agent.
Performance test: the elastic modulus G ' measured under its 200 μm of spacing of particle oil displacement agent made from embodiment 12=
7.023Pa；Viscosities il=the 15.78mPa.s measured under 1000 μm of spacing.
Embodiment 13
100 parts of acrylamides are dissolved in 150 parts of deionized water, aqueous solution is made and 1 part of crosslinking agent obtained is added
Solution A.It is 9 that 0.002 part of tetramethylethylenediamine, which is added, and adjusts solution pH value, is injected in adiabatic reaction kettle, at 12 DEG C of temperature,
After letting nitrogen in and deoxidizing 15 minutes, 0.05 part of potassium peroxydisulfate initiation reaction of 50 parts of water dissolution is added, carries out adiabatic polymerisation, it is solidifying to system
After glue, continuation is reacted 2 hours at 85 DEG C, by product chopping drying, is crushed, screening, is obtained particle oil displacement agent.
Performance test: the elastic modulus G ' measured under its 200 μm of spacing of particle oil displacement agent made from embodiment 13=
6.328Pa；Viscosities il=the 19.39mPa.s measured under 1000 μm of spacing.
Embodiment 14
100 parts of acrylamides are dissolved in 150 parts of deionized water, aqueous solution is made and 1 part of crosslinking agent obtained is added
Solution A.It is 9 that 0.002 part of tetramethylethylenediamine, which is added, and adjusts solution pH value, is injected in adiabatic reaction kettle, at 12 DEG C of temperature,
After letting nitrogen in and deoxidizing 15 minutes, 0.03 part of ammonium persulfate initiation reaction of 50 parts of water dissolution is added, carries out adiabatic polymerisation, it is solidifying to system
After glue, continuation is reacted 2 hours at 85 DEG C, by product chopping drying, is crushed, screening, is obtained particle oil displacement agent.
Performance test: the elastic modulus G ' measured under its 200 μm of spacing of particle oil displacement agent made from embodiment 14=
6.209Pa；Viscosities il=the 18.28mPa.s measured under 1000 μm of spacing.
Embodiment 15
100 parts of acrylamides are dissolved in 150 parts of deionized water, aqueous solution is made and 1 part of crosslinking agent obtained is added
H solution.It is 9 that 0.002 part of tetramethylethylenediamine, which is added, and adjusts solution pH value, is injected in adiabatic reaction kettle, at 12 DEG C of temperature,
After letting nitrogen in and deoxidizing 15 minutes, 0.03 part of potassium peroxydisulfate initiation reaction of 50 parts of water dissolution is added, carries out adiabatic polymerisation, it is solidifying to system
After glue, continuation is reacted 2 hours at 85 DEG C, by product chopping drying, is crushed, screening, is obtained particle oil displacement agent.
Performance test: the elastic modulus G ' measured under its 200 μm of spacing of particle oil displacement agent made from embodiment 15=
7.419Pa；Viscosities il=the 12.43mPa.s measured under 1000 μm of spacing.
Embodiment 16
100 parts of acrylamides are dissolved in 150 parts of deionized water, aqueous solution is made and 1 part of crosslinking agent obtained is added
I solution.It is 9 that 0.002 part of tetramethylethylenediamine, which is added, and adjusts solution pH value, is injected in adiabatic reaction kettle, at 12 DEG C of temperature,
After letting nitrogen in and deoxidizing 15 minutes, 0.03 part of potassium peroxydisulfate initiation reaction of 50 parts of water dissolution is added, carries out adiabatic polymerisation, it is solidifying to system
After glue, continuation is reacted 2 hours at 85 DEG C, by product chopping drying, is crushed, screening, is obtained particle oil displacement agent.
Performance test: the elastic modulus G ' measured under its 200 μm of spacing of particle oil displacement agent made from embodiment 16=
4.290Pa；Viscosities il=the 15.22mPa.s measured under 1000 μm of spacing.
Embodiment 17
100 parts of acrylamides are dissolved in 150 parts of deionized water, aqueous solution is made and 1 part of crosslinking agent obtained is added
J solution.It is 9 that 0.002 part of tetramethylethylenediamine, which is added, and adjusts solution pH value, is injected in adiabatic reaction kettle, at 12 DEG C of temperature,
After letting nitrogen in and deoxidizing 15 minutes, 0.03 part of potassium peroxydisulfate initiation reaction of 50 parts of water dissolution is added, carries out adiabatic polymerisation, it is solidifying to system
After glue, continuation is reacted 2 hours at 85 DEG C, by product chopping drying, is crushed, screening, is obtained particle oil displacement agent.
Performance test: the elastic modulus G ' measured under its 200 μm of spacing of particle oil displacement agent made from embodiment 17=
10.238Pa；Viscosities il=the 6.43mPa.s measured under 1000 μm of spacing.
Embodiment 18
100 parts of acrylamides are dissolved in 150 parts of deionized water, aqueous solution is made and 1 part of crosslinking agent obtained is added
K solution.It is 9 that 0.002 part of tetramethylethylenediamine, which is added, and adjusts solution pH value, is injected in adiabatic reaction kettle, at 12 DEG C of temperature,
After letting nitrogen in and deoxidizing 15 minutes, 0.03 part of potassium peroxydisulfate initiation reaction of 50 parts of water dissolution is added, carries out adiabatic polymerisation, it is solidifying to system
After glue, continuation is reacted 2 hours at 85 DEG C, by product chopping drying, is crushed, screening, is obtained particle oil displacement agent.
Performance test: the elastic modulus G ' measured under its 200 μm of spacing of particle oil displacement agent made from embodiment 18=
9.4568Pa；Viscosities il=the 8.93mPa.s measured under 1000 μm of spacing.
Claims (10)
1. a kind of POLYACRYLAMIDE FLOODING agent has the cross-linked network knot being centrally formed using polyfunctionality crosslinking agent as crosslinking
The polyacrylamide amine structure that structure and branching chain structure coexist, wherein cross-linked structure proportion in entire polyacrylamide amine structure
Be 60~95%, and the polyfunctionality crosslinking agent by allyl glycidyl ether or (methyl) glycidyl acrylate with
Polyethylene polyamine reaction and obtain.
2. POLYACRYLAMIDE FLOODING agent according to claim 1, wherein the polyethylene polyamine includes containing 2~4 Asias
The amine substance of ethyl and 2~5 primary amine or secondary amine group.
3. POLYACRYLAMIDE FLOODING agent according to claim 1 is gluey, particle or powdery.
4. POLYACRYLAMIDE FLOODING agent according to claim 1, aging 90 days in 85 DEG C, 30000 salinity salt water,
Still it is able to maintain 70% modulus.
5. a kind of method for preparing POLYACRYLAMIDE FLOODING agent according to claim 1, comprising the following steps:
(1) preparation of cross-linking agent solution: being the polyethylene polyamine and allyl glycidyl ether or (first of 1:2~5 by molar ratio
Base) glycidyl acrylate is soluble in water, so that the mass fraction of solute is 3-10%, then reacted at 50~85 DEG C,
Obtain polyfunctional crosslinking agent's solution；
(2) acrylamide polymerization reacts: being made aqueous solution for 100 parts of acrylamides are soluble in water, is added 0.5~5 part and has been made
Cross-linking agent solution；It is 8~10 that 0.002~0.04 part of organic amine, which is added, and adjusts solution ph；Gained reactant is added exhausted
In thermal response kettle, it is passed through inert gas deoxygenation, 0.03~0.05 part of persulfate initiation reaction is added at 5~30 DEG C of temperature,
Adiabatic polymerisation reaction is carried out under inert gas protection；After system gel, continuation is reacted 1~4 hour at 50-90 DEG C, is obtained
To the block-like POLYACRYLAMIDE FLOODING agent product of glue.
6. according to the method described in claim 5, wherein the polyethylene polyamine for being used to prepare crosslinking agent includes containing 2~4
The amine substance of a ethylidene and 2~5 primary amine or secondary amine group.
7. according to the method described in claim 5, wherein the reaction of step (1) carries out 5~7 hours.
8. according to the method described in claim 5, wherein the organic amine include aliphatic diamine, aliphatic tertiary amine or it
Mixture.
9. according to the method described in claim 5, wherein the inert gas includes nitrogen.
10. according to the method described in claim 5, further include by blob of viscose shape oil displacement agent product obtained chopping, drying, crush,
Screening, obtains particle or powdery oil displacement agent.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105154054A (en) * | 2015-08-07 | 2015-12-16 | 中国石油化工股份有限公司胜利油田分公司勘探开发研究院 | Cross-linked polymer flooding agent adopting triamine participating in synthesis and preparation method of cross-linked polymer flooding agent |
| CN109266322A (en) * | 2018-09-10 | 2019-01-25 | 四川大学 | A kind of polyacrylamide gel oil displacement agent and preparation method thereof with high tenacity |
-
2017
- 2017-07-07 CN CN201710552256.7A patent/CN109207137A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105154054A (en) * | 2015-08-07 | 2015-12-16 | 中国石油化工股份有限公司胜利油田分公司勘探开发研究院 | Cross-linked polymer flooding agent adopting triamine participating in synthesis and preparation method of cross-linked polymer flooding agent |
| CN109266322A (en) * | 2018-09-10 | 2019-01-25 | 四川大学 | A kind of polyacrylamide gel oil displacement agent and preparation method thereof with high tenacity |
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