CN104357039B - A kind of polymer microballoon emulsion oil displacement agent and preparation method thereof - Google Patents
A kind of polymer microballoon emulsion oil displacement agent and preparation method thereof Download PDFInfo
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- 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
- C08F2/00—Processes of polymerisation
- C08F2/12—Polymerisation in non-solvents
- C08F2/16—Aqueous medium
- C08F2/22—Emulsion polymerisation
- C08F2/24—Emulsion polymerisation with the aid of emulsifying agents
- C08F2/26—Emulsion polymerisation with the aid of emulsifying agents anionic
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- C—CHEMISTRY; METALLURGY
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/12—Polymerisation in non-solvents
- C08F2/16—Aqueous medium
- C08F2/22—Emulsion polymerisation
- C08F2/24—Emulsion polymerisation with the aid of emulsifying agents
- C08F2/30—Emulsion polymerisation with the aid of emulsifying agents non-ionic
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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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- 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
- C09K8/584—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 surfactants
Abstract
The present invention relates to a kind of polymer microballoon emulsion oil displacement agents and preparation method thereof.A kind of polymer microballoon emulsion oil displacement agent, is mixed by surfactant, acrylamide, Ludox, crosslinking agent, potassium peroxydisulfate, sodium sulfite, white oil.A kind of preparation method of polymer microballoon emulsion oil displacement agent includes the following steps：（1）Aqueous phase solution is prepared；（2）Microemulsion system to be polymerized is prepared；（3）Polymerization crosslinking reacts.The polymer microballoon emulsion oil displacement agent of the present invention reaches 10 with mixed dehydration crude oil oil water interfacial tension‑3MN/m ranks, 50 210nm of microspherulite diameter distribution, expansion multiple reach 12 times of own wt, 100 DEG C of heatproof, salt tolerant 20 × 104Mg/L, it is stifled and reduce oil water interfacial tension ability to be provided simultaneously with tune, solves single note surfactant and does not have washing oil ability, polymer microballoon and surfactant there are channelling, existing polymer microballoon and directly compound the uncertain defect of synergy.
Description
Technical field
The present invention relates to a kind of oil displacement agents used for tertiary oil recovery and preparation method thereof, and in particular to a kind of polymer microballoon lotion
Oil displacement agent and preparation method thereof belongs to Oilfield Chemicals synthesis technical field.
Background technology
Chemical flooding is the technical way for continuing to improve recovery ratio the waterflooding development oil field later stage, studies at home and abroad show that table
Face surfactant flooding oil increasing effect is notable, with temperature-resistant anti-salt surfactant research and development success, be high temperature, with high salt and high contents of calcium and magnesium from
The selection that seed oil hides tertiary oil recovery mode provides new approaches.For Heterogeneous Reservoirs, single note surfactant, which exists, alters
The surfactant of flow problem, the predominant pathway channelling that surfactant is formed along water drive, injection forms inefficient cycle, involves body
Product substantially reduces, and improves recovery ratio limited extent.Therefore, fluidity control how is carried out as the application of surfactant flooding technology
Key technical problem.
Polymer microballoon due to water-swellable, compressional deformation, absorption characteristic, in injecting migration process realize envelope
Stifled formation pore throat, breakthrough, the profile control characteristic step by step goed deep into, blocked again, the selectivity water suction of hydrogel microsphere and super-strong moisture absorbing are swollen
Swollen characteristic is especially suitable for the closure of flow predominant pathway, realizes liquid stream changed course, and after pressure difference of blocking is more than certain value, microballoon can be sent out
Raw elastic deformation and continue, toward deep migration, to play a part of along journey profile control by pore throat, laboratory experiment show polymer microballoon and
There is good fluidity control effect after surfactant compounding, can effectively solve the problems, such as channelling existing for single note surfactant.
Application No. is 200910256126.4 patent application, to disclose a kind of low interfacial tension polyacrylamide nano micro-
The preparation method of ball transfer drive system reacts the sulfonic acid for generating high activity by the organic acid substance of the addition in emulsifier with alkali
Oil water interfacial tension is greatly lowered in salt or carboxylate surfactant, the reservoir condition in the oil recovery factories Shengli Oil Field Zhuan Xi
Under determine the case where system reduces the oil water interfacial tension of crude oil, performance is not carried out for polymer microballoon system and is commented
Valence, it is even more impossible to judge for adaptability and transfer drive situation for higher temperature salinity；ZL201110130518.3 discloses one kind
Natural carboxylate-polymer microballoon binary composite control system is compounded to obtain and can shown by microballoon with red yolk duck egg
Writing reduces oil water interfacial tension, improves the binary compound displacement system of washing oil ability.
Reverse microemulsion polymerization prepares polymer microballoon and needs to use a large amount of emulsifier, typically constitutes from system gross mass
15% or more, a large amount of emulsifiers of addition make production cost greatly improve, and take a broad view of existing document and patent, and reverse micro emulsion is poly-
It is mostly lipophilic surfactant Span series and hydrophilic surfactant active Tween series, OP series to close the emulsifier used
Composite emulsifier, when polymer microballoon lotion is made into aqueous solution injection oil reservoir after, these conventional emulsifiers used are not
Having, which reduces oil water interfacial tension, improves displacement efficiency ability, causes huge waste.
In conclusion single note surfactant fluidity control scarce capacity；Single polymer injection microballoon reduces oil-water interfaces
Power scarce capacity；Polymer microballoon directly compounds synergistic in the presence of uncertain with surfactant.
Invention content
It is an object of the invention to overcome channelling, polymer microballoon existing for single note surfactant not to have washing oil energy
Power, polymer microballoon and surfactant directly compound synergistic uncertain defect, provide a kind of polymer microballoon lotion
Oil displacement agent.
It is a further object to provide the preparation methods of above-mentioned oil displacement agent.
The invention is realized by the following technical scheme：
A kind of polymer microballoon emulsion oil displacement agent, by surfactant, acrylamide, Ludox, crosslinking agent, persulfuric acid
Potassium, sodium sulfite, white oil are mixed by following mass percent：The surfactant of 20%-30%, the third of 20%-30%
Acrylamide, the Ludox of 0.5%-3%, the crosslinking agent of 0.1%-0.5%, the potassium peroxydisulfate of 0.1%-0.5%, 0.1%-
0.5% sodium sulfite, the white oil of 25%-35%, surplus are deionized water, contain structural formula shown in formula 1, formula 2：
In formula 1, R1For C8-C18Alkyl；
In formula 2, R2For alkyl or alkylene, R3For methyl, ethyl, propyl or ethoxy.
A kind of preparation method of polymer microballoon emulsion oil displacement agent includes the following steps：
(1) aqueous phase solution is prepared：Deionized water is first added in the reaction vessel, based on gross mass 100%, it is dense that quality is added
Degree is the crosslinking agent of the acrylamide of 20%-30%, the Ludox of 0.5%-3%, 0.1%-0.5%, is mixed and dissolved into
Clear solution；
(2) microemulsion system to be polymerized is prepared：Based on gross mass 100%, sequentially add 25%-35%'s in a kettle
The surfactant of white oil and 20%-30%, it is to be mixed to after being completely dissolved uniformly, under the mixing speed of 300-400r/min
It is slowly added to the aqueous phase solution that step (1) obtains, is sufficiently stirred, a kind of transparent or semitransparent microemulsion to be polymerized reaction is obtained
System；
(3) polymerization crosslinking reacts：The potassium peroxydisulfate of 0.1%-0.5% is added in the microemulsion to be polymerized of step (2),
After stirring evenly, it is passed through inert gas replacement in a kettle and goes out oxygen, adjusts reaction temperature to 20-40 DEG C, with 300-400r/
Min speed stirs and is added the sodium sulfite initiated polymerization of 0.1%-0.5%, and after waiting for peak heat release, the reaction was continued
0.5-2 hours to get to a kind of transparent or semitransparent, thermodynamically stable low interfacial tension polymer microballoon emulsion flooding oil body
System；
(4) in the product that step (3) obtains, continue the addition step (1) under the mixing speed of 300-400r/min and obtain
The aqueous phase solution arrived obtains a kind of new microemulsion reaction system to be polymerized, then the repeatedly polymerization crosslinking reaction of step (3),
It can be obtained the low interfacial tension polymer microballoon lotion with higher polymer microballoon concentration.
The surfactant is the mixing of alkanolamide, sorbester p17, Cocoamidopropyl betaine and small molecular alcohol
Object, and mass ratio of each component is 6:3:0.8:0.2.
The alkanolamide be lauric acid diethyl amide, myristic acid diglycollic amide, Stearic acid diethanolamine salt,
One or both of lauric acid amide of ethanol, oleic acid diethyl amide.
The small molecular alcohol is one or both of methanol, ethyl alcohol, isopropanol.
The crosslinking agent is the mixture for going back oxygen chloropropane and methene base bisacrylamide, mass ratio 1:9.
The inert gas is one kind in nitrogen, helium, argon gas.
The beneficial effects of the invention are as follows：A kind of low interfacial tension polymer microballoon emulsion oil displacement agent, with mixed dehydration crude oil
Oil water interfacial tension reaches 10-3MN/m ranks, microspherulite diameter distribution 50-210nm, expansion multiple reach 12 times of own wt,
100 DEG C of heatproof, salt tolerant 20 × 104Mg/L can be applied to high temperature and high salinity reservoir condition；It is provided simultaneously with tune and blocks up and reduce oil
Water interfacial tension ability, solving single note surfactant, there are channelling, existing polymer microballoons not to have washing oil ability, polymerization
Object microballoon directly compounds synergistic uncertain defect with surfactant.
Description of the drawings
Attached drawing 1 is 1 products obtained therefrom initial particle distribution map of the embodiment of the present invention；
Attached drawing 2 is 2 products obtained therefrom initial particle distribution map of the embodiment of the present invention；
Attached drawing 3 is embodiment 1 and 2 products obtained therefrom of embodiment and the eastern mixed dehydration crude oil interfacial tension comparison diagram of text 25.
Specific implementation mode
With reference to embodiment, the following further describes the technical solution of the present invention.
Embodiment 1：
25g acrylamides are dissolved in 21.07g deionized waters in the reaction vessel, are stirred well to solution clarification without solid
Body insoluble matter sequentially adds 0.09g methene bases bisacrylamide, 0.1g epoxychloropropane, 0.12g Ludox, is stirred
It is dissolved into clear solution；30g white oils, 13g lauric acid amide of ethanol, 6.5g sorbester p17s, 1.7g are sequentially added in a kettle
Cocoamidopropyl betaine, 0.4g ethyl alcohol, 0.03g isopropanols, stirring are stirred to after being completely dissolved uniformly in 300-400r/min
The clear solution being gradually added under speed in reaction vessel is mixed, is sufficiently stirred, is obtained a kind of transparent or semitransparent to be polymerized micro-
Lotion；0.1g potassium peroxydisulfates are added in the microemulsion to be polymerized in reaction kettle, after stirring evenly, are passed through nitrogen in a kettle
Gas 10min, temperature are adjusted to 30 DEG C, and 0.1g sodium sulfite initiated polymerizations are stirred and be added with 300-400r/min speed,
After waiting for peak heat release, the reaction was continued 1h is to get being the transparent or semitransparent thermodynamics of 80-180nm to a kind of microballoon initial particle
Stable low interfacial tension polymer microballoon lotion oil displacement system, particle diameter distribution are as shown in Figure 1.
Embodiment 2：
30g acrylamides are dissolved in 18.7g deionized waters in the reaction vessel, are stirred well to solution clarification without solid
Insoluble matter, sequentially adding 0.27g methenes base, acrylamide, 0.03g epoxychloropropane, 0.5g Ludox are stirred dissolving again
At clear solution；25g white oils, 15g lauric acid amide of ethanol, 7.5g sorbester p17s, 2g cocounut oil acyls are sequentially added in a kettle
Amine propyl betaine, 0.5g isopropanols are added by 1 identical condition of embodiment and step method in 2/3rds reaction vessels
Clear solution obtains microemulsion reaction system to be polymerized；0.15g potassium peroxydisulfates are added in microemulsion to be polymerized, stirring is equal
After even, it is passed through nitrogen 10min in a kettle, temperature is adjusted to 20 DEG C, is stirred with 300-400r/min speed and 0.15g is added
Sodium sulfite initiated polymerization, after waiting for peak heat release, the reaction was continued 1h continues to be added with identical mixing speed after cooling
Remaining one third clear solution in reaction vessel, by above-mentioned identical condition and step method be added 0.08g potassium peroxydisulfates,
After 0.08g sodium sulfites initiated polymerization to get to a kind of microballoon initial particle be the transparent or semitransparent heating power of 50-150nnm
Stable low interfacial tension polymer microballoon lotion oil displacement system is learned, particle diameter distribution is as shown in Figure 2.
3~8 step of embodiment is identical as embodiment 1 or 2, and drug proportioning used is as shown in table 1：
Drug used in 1 embodiment 3~8 of table matches table
Use total salinity for 20 × 10 the product that embodiment 1- embodiments 2 obtain4The live water of mg/l is configured to dense
Degree is measured with rotation drop ultralow interfacial tension instrument TX500C in for 0.5% solution under the conditions of 85 DEG C and 6000r/min
The oil water interfacial tension of 25 east dehydration mixed crude of crude oil field text reaches 10-3Following rank illustrates the present invention as shown in Fig. 3
Oil displacement efficiency can be effectively improved.
The product that embodiment 1- embodiments 8 obtain is configured to the molten of a concentration of 0.3%-2% using above-mentioned same method
Liquid measures oil water interfacial tension as stated above, and the initial grain of product is measured using 3000 particle size analyzer of Britain's Malvern
Diameter is distributed, and the results are shown in Table 2.
A concentration of 0.5% solution of above-mentioned preparation is put in 100 DEG C of baking ovens, above-mentioned similarity condition is used after 30 days
Method measures oil water interfacial tension；The particle diameter distribution for measuring product with particle size analyzer at regular intervals, as a result such as table 2.
A kind of 2 low interfacial tension polymer microballoon emulsion oil displacement agent performance of table and high-temperature stability
The low interfacial tension polymer microballoon lotion that it can be seen from table 1-2 and attached drawing 1-3 prepared by the present invention and middle original text
25 eastern block mixed dehydration crude oil form ultralow interfacial tension, and microballoon initial particle is Nano grade, has good temperature-resistant anti-salt
Property, brine swelliong power, delayed expansion performance and high-temperature stability are inhaled, polymer microballoon tune is had both and blocks up and surfactant reduction
The dual property of oil water interfacial tension disclosure satisfy that the needs of high temperature and high salt oil deposit chemical flooding.
Claims (11)
1. a kind of polymer microballoon emulsion oil displacement agent, it is characterized in that：Using reverse microemulsion polymerization by surfactant, acryloyl
Amine, Ludox, crosslinking agent, potassium peroxydisulfate, sodium sulfite, white oil are made by following mass percent：It lives on the surface of 20%-30%
Property agent, the acrylamide of 20%-30%, the Ludox of 0.5%-3%, the crosslinking agent of 0.1%-0.5%, 0.1%-0.5%
Potassium peroxydisulfate, the sodium sulfite of 0.1%-0.5%, the white oil of 25%-35%, surplus are deionized water；
The surfactant contains structural formula shown in formula 1 and formula 2：
In formula 1, R1For C8-C18Alkyl；
In formula 2, R2For alkyl or alkylene, R3For methyl, ethyl, propyl or ethoxy.
2. polymer microballoon emulsion oil displacement agent according to claim 1, it is characterized in that：The surfactant is alkanol
The mixture of amide, sorbester p17, Cocoamidopropyl betaine and small molecular alcohol, and mass ratio of each component is 6:3:0.8:0.2.
3. polymer microballoon emulsion oil displacement agent according to claim 2, it is characterized in that：The alkanolamide is lauric acid
Diglycollic amide, myristic acid diglycollic amide, Stearic acid diethanolamine salt, lauric acid amide of ethanol, oleic acid diethanol acyl
One or both of amine.
4. polymer microballoon emulsion oil displacement agent according to claim 2, it is characterized in that：The small molecular alcohol be methanol,
One or both of ethyl alcohol, isopropanol.
5. polymer microballoon emulsion oil displacement agent according to claim 1, it is characterized in that：The crosslinking agent is to go back oxygen chlorine third
The mixture of alkane and methene base bisacrylamide, mass ratio 1:9.
6. a kind of preparation method of polymer microballoon emulsion oil displacement agent as described in claim 1, includes the following steps：
(1) aqueous phase solution is prepared：Deionized water is first added in the reaction vessel, based on gross mass 100%, mass concentration, which is added, is
The crosslinking agent of the acrylamide of 20%-30%, the Ludox of 0.5-3%, 0.1%-0.5% is mixed and dissolved into transparent molten
Liquid；
(2) microemulsion system to be polymerized is prepared：Based on gross mass 100%, the white oil of 25%-35% is sequentially added in a kettle
It is to be mixed to after being completely dissolved uniformly with the surfactant of 20%-30%, then with slow under 300-400r/min mixing speeds
The aqueous phase solution that step (1) obtains is added, is sufficiently stirred, obtains a kind of transparent or semitransparent microemulsion reactant to be polymerized
System；
(3) polymerization crosslinking reacts：The potassium peroxydisulfate of 0.1%-0.5% is added in the microemulsion to be polymerized of step (2), is stirred
After uniformly, it is passed through inert gas replacement in a kettle and goes out oxygen, adjusts reaction temperature to 20-40 DEG C, with 300-400r/min
Speed stirs and the sodium sulfite initiated polymerization of 0.1%-0.5% is added, after waiting for peak heat release, the reaction was continued 0.5-2
Hour to get to a kind of transparent or semitransparent, thermodynamically stable low interfacial tension polymer microballoon lotion oil displacement system；
(4) in step (3) obtains product, continue that step (1) obtained aqueous phase solution is added under stiring, obtain a kind of new
Microemulsion reaction system to be polymerized repeats the polymerization crosslinking reaction of step (3), you can obtain with higher polymer microballoon concentration
Low interfacial tension polymer microballoon lotion.
7. the preparation method of polymer microballoon emulsion oil displacement agent according to claim 6, it is characterized in that：It lives on the surface
Property agent be alkanolamide, sorbester p17, Cocoamidopropyl betaine and small molecular alcohol mixture, and mass ratio of each component be 6:
3:0.8:0.2。
8. the preparation method of polymer microballoon emulsion oil displacement agent according to claim 7, it is characterized in that：The alkanol acyl
Amine is lauric acid diethyl amide, myristic acid diglycollic amide, Stearic acid diethanolamine salt, lauric acid amide of ethanol, oil
One or both of sour diglycollic amide.
9. the preparation method of polymer microballoon emulsion oil displacement agent according to claim 7, it is characterized in that：The small molecule
Alcohol is one or both of methanol, ethyl alcohol, isopropanol.
10. the preparation method of polymer microballoon emulsion oil displacement agent according to claim 6, it is characterized in that：The crosslinking
Agent is to go back the mixture of oxygen chloropropane and methene base bisacrylamide, mass ratio 1:9.
11. the preparation method of polymer microballoon emulsion oil displacement agent according to claim 6, it is characterized in that：The inertia
Gas is one kind in nitrogen, helium, argon gas.
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| CN109666473A (en) * | 2017-10-17 | 2019-04-23 | 中国石油化工股份有限公司 | Surfactant binary built flooding method |
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