CN106749921A - A kind of transfer drive grafting polymer microballoon and preparation method thereof - Google Patents
A kind of transfer drive grafting polymer microballoon and preparation method thereof Download PDFInfo
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- CN106749921A CN106749921A CN201611020315.8A CN201611020315A CN106749921A CN 106749921 A CN106749921 A CN 106749921A CN 201611020315 A CN201611020315 A CN 201611020315A CN 106749921 A CN106749921 A CN 106749921A
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F251/00—Macromolecular compounds obtained by polymerising monomers on to polysaccharides or derivatives thereof
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- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/50—Compositions for plastering borehole walls, i.e. compositions for temporary consolidation of borehole walls
- C09K8/504—Compositions based on water or polar solvents
- C09K8/506—Compositions based on water or polar solvents containing organic compounds
- C09K8/508—Compositions based on water or polar solvents containing organic compounds macromolecular compounds
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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
- C09K8/50—Compositions for plastering borehole walls, i.e. compositions for temporary consolidation of borehole walls
- C09K8/516—Compositions for plastering borehole walls, i.e. compositions for temporary consolidation of borehole walls characterised by their form or by the form of their components, e.g. encapsulated material
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Abstract
The present invention relates to a kind of oil well profile-controlling and plugging agent, more particularly to a kind of transfer drive grafting polymer microballoon and preparation method thereof.Each constituent and its mass ratio of the polymer microsphere be：Etherification starch：Acrylamide：N, N methylene-bisacrylamide：Ammonium persulfate=1~2：0.5~1.5：0.04~0.2：0.1~0.5.Polymer microsphere of the invention have the advantages that good size tunable, homogeneity, high temperature resistant good salt tolerance, raw material sources extensively, low cost of manufacture, will not be hydrolyzed in harsh salt environment, and it is degradable, spherex further can go deep into inside oil reservoir after water absorption and swelling, the microballoon of polymerization has the rigidity characteristic of starch polymer and the flexible variable characteristic of acrylamide concurrently simultaneously, it is hard and soft successive, go deep into and sealing characteristics with preferable, it is environmentally safe, rock stratum anisotropism is reduced, oil recovery factor is improved.
Description
Technical field：
The present invention relates to a kind of oil well profile-controlling and plugging agent, more particularly to a kind of transfer drive grafting polymer microballoon and its system
Preparation Method.
Background technology：
In the middle and later periods of oil field development, due to the presence of formation heterogeneity, waterflooding extraction process no matter in plane or
Water drive propulsion is all uneven on longitudinal direction, and the clay swell that causes by long-term current scour in addition, fine migration shake out, and enter one
Step causes anisotropism to deteriorate, and some oil reservoir positions form macropore even extra big channel, cause the Thief zone between injection-production well
Layer is prematurely formed water logging, reduces injection water and involves degree to less permeable layer, causes the aqueous rising of surrounding oil well, or even water
Flood, cause the oil of some less permeable layers to be exploited not out.Therefore in the water flooding middle and later periods, Thief zone ground can be blocked
Layer, the own important measures that oil recovery factor is improved through turning into of oilwell water shutoff and Profile Control in Injection Well for improving sweep area.Additionally, with
Deepening continuously for water flooding, downhole conditions are deteriorated year by year, many traditional card envelopes are made to realize already, at this
Chemistry adjusts stifled advantage just more and more obvious in the case of kind.Therefore, the research of profile-controlling and plugging agent in the last few years is received with application
Extensive concern.
The chemical plugging agent mainly low concentration partially hydrolyzed polyacrylamide (PHPA) that current oil field often uses exists with aluminium citrate
Mobility gel, Weak Gels, linked polymer coil that cross-linked polymeric is formed under different condition etc., but this kind of plugging agent is due to receiving
The influence of the factors such as polyacrylamide high temperature degradation, high salt high shear viscosity reduction, it is existing under the conditions of oilfield sewage and reservoir temperature etc.
Prepare or in the plugging agent poor-performing of underground polymerization generation, even cannot form cross-linked polymer sometimes in field.Therefore, it is badly in need of
Develop a kind of tune that still be can guarantee that under conditions of high temperature and high salt inside enough intensity, not degradable, deep enough oil reservoir
Blocking agent.
The content of the invention：
The technical problem to be solved in the present invention is to provide a kind of transfer drive grafting polymer microballoon and preparation method thereof, the height
Molecule microballoon realizes extensive, low cost of manufacture with size tunable, good homogeneity, high temperature resistant good salt tolerance, raw material sources
Advantage, will not hydrolyze in harsh salt environment, and not degradable, and spherex can further go deep into oil after water absorption and swelling
Layer is internal, while the microballoon of polymerization has the rigidity characteristic of starch polymer and the flexible variable characteristic of acrylamide, hard and soft phase concurrently
After, go deep into and sealing characteristics with preferable, it is environmentally safe, rock stratum anisotropism is reduced, improve oil recovery factor.Overcome
Existing plugging agent low intensity under conditions of high temperature and high salt, poor performance is degraded, it is impossible to inside deep enough oil reservoir not
Foot.
The technical solution used in the present invention is：A kind of transfer drive grafting polymer microballoon, each group of the polymer microsphere
It is into composition and its mass ratio：Etherification starch：Acrylamide：N, N- methylene-bisacrylamide：Ammonium persulfate=1~2：0.5
~1.5：0.04~0.2：0.1~0.5.
A kind of transfer drive preparation method of grafting polymer microballoon, the method step is as follows：
First, prepared by aqueous phase solution：The etherification starch of 1~2 mass fraction is taken, deionized water is added, pH value to 8 is adjusted,
0.5h is gelatinized in 80 DEG C of thermostat water baths, after being gelatinized in the acrylamide addition thermostat water bath for weighing 0.5~1.5 mass fraction
Solution in, regulation aqueous phase solution volume is n, and etherification starch concentration is 50000~100000mg/L, water phase in making aqueous phase solution
The concentration of acrylamide is 25000~75000mg/L in solution；
2nd, prepared by oil-phase solution：Oil phase solvent is added in 60 DEG C of thermostat water baths, oil phase solvent is by 4 volume parts
The chloroform composition of hexamethylene and 1 volume parts, adds the composite emulsifier of 1~2 mass fraction in oil phase solvent, wherein
Composite emulsifier is formed by the Tween60 compoundings of 9 Span60 and 1 of mass fraction mass fractions, on thermostat water bath
Load onto electric mixer and condensation reflux unit, under 60 DEG C of waters bath with thermostatic control stirring dissolve composite emulsifier to be made oil phase molten
Liquid, compound emulsion agent concentration is 10000~20000mg/L in oil-phase solution；
3rd, synthetic reaction：The N of 0.04~0.2 mass fraction, N- methylene-bisacrylamides are added in aqueous phase solution,
Magnetic agitation makes N, and the dissolving of N- methylene-bisacrylamides makes N in aqueous phase solution, and N- methylene-bisacrylamides concentration is 2000
~10000mg/L, then the ammonium persulfate of 0.1~0.5 mass fraction is added in aqueous phase solution, ammonium persulfate is dense in aqueous phase solution
It is 5000~25000mg/L to spend, and now aqueous phase solution and the volume ratio of oil-phase solution are 1/5~1/3, will after ammonium persulfate dissolving
Aqueous phase solution is added dropwise in oil-phase solution, is dripped off in 5min, is first kept the rotating speed of 900r/min to stir 5min after dripping off and is formed instead
To emulsion system, rotating speed stirring water bath with thermostatic control A DEG C of reaction 2~3h, 50 DEG C≤A DEG C≤60 DEG C of 600r/min are then changed to；
4th, product treatment：Reaction is poured into beaker product after terminating, and it is the absolute ethyl alcohol of 1.5*n, magnetic force to add volume
Stirring 0.5h, discards supernatant liquor, adds the acetone that volume is 0.75n~n, is dried under normal temperature, collects white powder and is
This product.
The beneficial effects of the invention are as follows：There is the present invention size tunable, good homogeneity, high temperature resistant good salt tolerance, raw material to come
Source is extensive, the advantage of low cost of manufacture, will not be hydrolyzed in harsh salt environment, and not degradable, and spherex is molten in water suction
Further can go deep into inside oil reservoir after swollen, while the microballoon of polymerization has the rigidity characteristic and acrylamide of starch polymer concurrently
Flexible variable characteristic, it is hard and soft to go deep into and sealing characteristics with preferable in succession, it is environmentally safe, rock stratum anisotropism is reduced,
Improve oil recovery factor.
Brief description of the drawings：
The present invention will be further described in detail with reference to the accompanying drawings and detailed description.
Fig. 1 is transfer drive grafting polymer microspheres solution filling sandpipe experiment closure curve.
Specific embodiment：
A kind of transfer drive grafting polymer microballoon, each constituent and its mass ratio of the polymer microsphere are：Etherificate is formed sediment
Powder：Acrylamide：N, N- methylene-bisacrylamide：Ammonium persulfate=1~2：0.5~1.5：0.04~0.2：0.1~0.5.
A kind of transfer drive preparation method of grafting polymer microballoon, the method step is as follows：
First, prepared by aqueous phase solution：The etherification starch of 1~2 mass fraction is taken, deionized water is added, pH value to 8 is adjusted,
0.5h is gelatinized in 80 DEG C of thermostat water baths, after being gelatinized in the acrylamide addition thermostat water bath for weighing 0.5~1.5 mass fraction
Solution in, regulation aqueous phase solution volume is n, and etherification starch concentration is 50000~100000mg/L, water phase in making aqueous phase solution
The concentration of acrylamide is 25000~75000mg/L in solution；
2nd, prepared by oil-phase solution：Oil phase solvent is added in 60 DEG C of thermostat water baths, oil phase solvent is by 4 volume parts
The chloroform composition of hexamethylene and 1 volume parts, adds the composite emulsifier of 1~2 mass fraction in oil phase solvent, wherein
Composite emulsifier is formed by the Tween60 compoundings of 9 Span60 and 1 of mass fraction mass fractions, on thermostat water bath
Load onto electric mixer and condensation reflux unit, under 60 DEG C of waters bath with thermostatic control stirring dissolve composite emulsifier to be made oil phase molten
Liquid, compound emulsion agent concentration is 10000~20000mg/L in oil-phase solution；
3rd, synthetic reaction：The N of 0.04~0.2 mass fraction, N- methylene-bisacrylamides are added in aqueous phase solution,
Magnetic agitation makes N, and the dissolving of N- methylene-bisacrylamides makes N in aqueous phase solution, and N- methylene-bisacrylamides concentration is 2000
~10000mg/L, then the ammonium persulfate of 0.1~0.5 mass fraction is added in aqueous phase solution, ammonium persulfate is dense in aqueous phase solution
It is 5000~25000mg/L to spend, and now aqueous phase solution and the volume ratio of oil-phase solution are 1/5~1/3, will after ammonium persulfate dissolving
Aqueous phase solution is added dropwise in oil-phase solution, is dripped off in 5min, is first kept the rotating speed of 900r/min to stir 5min after dripping off and is formed instead
To emulsion system, rotating speed stirring water bath with thermostatic control A DEG C of reaction 2~3h, 50 DEG C≤A DEG C≤60 DEG C of 600r/min are then changed to；
4th, product treatment：Reaction is poured into beaker product after terminating, and it is the absolute ethyl alcohol of 1.5*n, magnetic force to add volume
Stirring 0.5h, discards supernatant liquor, adds the acetone that volume is 0.75n~n, is dried under normal temperature, collects white powder and is
This product.
The spherex of different-grain diameter and intensity is can obtain in the present invention by changing different reactant ratios.Synthesis is produced
Product are white powder, stir water-soluble, the white emulsion of the aqueous solution.Infrared spectrum detection is carried out to sample can be found significantly
The flexural vibrations peak of acid amides N-H, tertiary amine C-N stretching vibration peaks, illustrate etherification starch, acrylamide and N, N- methylene bisacrylamide
Acid amides there occurs cross-linking reaction, can be found with the microballoon in the observation by light microscope aqueous solution, microballoon graininess spherical in shape, particle diameter
It it is 50~150 μm, the swelling ratio that may be such that microballoon with salt in aqueous increases.
Evaluated with the sealing characteristics of grafting polymer microspheres product being prepared as described above transfer drive obtained in method：Using
Physical model experiment carrys out the sealing characteristics of evaluation starch microballoon, 1000ppm, this product solution of 4000 salinities is prepared, through filling
Point stirring after be placed in it is swelling stand-by in 45 DEG C of insulating boxs.From the quartz sand of different meshes, the filling that length is 100cm is filled into
In sandpipe, filling sandpipe is placed in 45 DEG C of insulating boxs, filling sandpipe 48h is washed away with stratum water, simulation long-term injecting water exploitation
Stratum, it is 1.5D to determine filling sandpipe permeability.This product solution is clamp-oned with the flow of 0.4L/min by sandpipe, record sandpipe is each
The pressure changing of pressure tap.Experimental result draws, this product solution for 1000ppm, with the increase of injected slurry volume,
Each pressure tap pressure oscillation of sandpipe rises；As shown in figure 1, when injected slurry volume reaches 4.0Vp, along three pressure measurement of grain direction
Point pressure rises to 29.8KPa, 17.3KPa, 10.5KPa by 6.8KPa, 5.7KPa, 5.6KPa respectively.Note this product solution is complete
After finishing metaideophone stratum water, pressure declines a little.Result illustrates that it is 1.5D's that this product solution of 1000ppm can penetrate deep into rate
Filling sandpipe simultaneously forms good closure to sandpipe.
Current this product has been carried out multigroup closure and the experiment of transfer drive Lab-evaluation, test result indicate that, transfer drive is with connecing
Branch polymer microsphere could be formed with effect closure, and can enter stratum depths, and residual resistive higher can also be kept after turning water drive
Coefficient, is a kind of preferably new transfer drive plugging material.
It is understood that above with respect to specific descriptions of the invention, being merely to illustrate the present invention and being not limited to this
Technical scheme described by inventive embodiments, it will be understood by those within the art that, still the present invention can be carried out
Modification or equivalent, to reach identical technique effect；As long as satisfaction use needs, all protection scope of the present invention it
It is interior.
Claims (2)
1. a kind of transfer drive grafting polymer microballoon, it is characterised in that：Each constituent and its mass ratio of the polymer microsphere
For：Etherification starch：Acrylamide：N, N- methylene-bisacrylamide：Ammonium persulfate=1~2：0.5~1.5：0.04~0.2：
0.1~0.5.
2. a kind of transfer drive according to described in claim 1 preparation method of grafting polymer microballoon, it is characterised in that：The method
Step is as follows：
First, prepared by aqueous phase solution：The etherification starch of 1~2 mass fraction is taken, deionized water is added, pH value is adjusted to 8, at 80 DEG C
0.5h is gelatinized in thermostat water bath, it is molten after being gelatinized in the acrylamide addition thermostat water bath for weighing 0.5~1.5 mass fraction
In liquid, regulation aqueous phase solution volume is n, and etherification starch concentration is 50000~100000mg/L, aqueous phase solution in making aqueous phase solution
The concentration of middle acrylamide is 25000~75000mg/L；
2nd, prepared by oil-phase solution：In 60 DEG C of thermostat water baths add oil phase solvent, oil phase solvent by 4 volume parts hexamethylene
The chloroform composition of alkane and 1 volume parts, adds the composite emulsifier of 1~2 mass fraction, wherein compounding in oil phase solvent
Emulsifying agent is formed by the Tween60 compoundings of 9 Span60 and 1 of mass fraction mass fractions, is loaded onto on thermostat water bath
Electric mixer and condensation reflux unit, stirring makes composite emulsifier dissolving be made oil-phase solution under 60 DEG C of waters bath with thermostatic control, oil
Compound emulsion agent concentration is 10000~20000mg/L in phase solution；
3rd, synthetic reaction：The N of 0.04~0.2 mass fraction, N- methylene-bisacrylamides are added in aqueous phase solution, magnetic force
Stirring makes N, the dissolving of N- methylene-bisacrylamides, makes N in aqueous phase solution, and N- methylene-bisacrylamides concentration is 2000~
10000mg/L, then the ammonium persulfate of 0.1~0.5 mass fraction, ammonium persulfate concentrations in aqueous phase solution are added in aqueous phase solution
It is 5000~25000mg/L, now aqueous phase solution and the volume ratio of oil-phase solution are 1/5~1/3, by water after ammonium persulfate dissolving
The drop that mixes is added in oil-phase solution, is dripped off in 5min, is first kept the rotating speed of 900r/min to stir 5min after dripping off and is formed reversely
Emulsion system, is then changed to rotating speed stirring water bath with thermostatic control A DEG C of reaction 2~3h, 50 DEG C≤A DEG C≤60 DEG C of 600r/min；
4th, product treatment：Reaction is poured into beaker product after terminating, and it is the absolute ethyl alcohol of 1.5*n, magnetic agitation to add volume
0.5h, discards supernatant liquor, adds the acetone that volume is 0.75n~n, is dried under normal temperature, collects white powder and is this product
Product.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2019037743A1 (en) * | 2017-08-22 | 2019-02-28 | 中国石油化工股份有限公司 | Starch-containing microsphere and preparation method therefor and application thereof |
| CN109422887A (en) * | 2017-08-22 | 2019-03-05 | 中国石油化工股份有限公司 | A kind of anionic starch microballoon and its preparation method and application |
| CN109422886A (en) * | 2017-08-22 | 2019-03-05 | 中国石油化工股份有限公司 | A kind of anion doped spherex material and its preparation method and application |
| CN109422852A (en) * | 2017-08-22 | 2019-03-05 | 中国石油化工股份有限公司 | A kind of micron order spherex and its preparation method and application |
| CN109422851A (en) * | 2017-08-22 | 2019-03-05 | 中国石油化工股份有限公司 | A kind of cationic starch microballoon and its preparation method and application |
| CN112708011A (en) * | 2019-10-25 | 2021-04-27 | 中国石油化工股份有限公司 | Novel negative and positive composite flexible polymer microsphere and preparation method thereof |
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| CN104017131A (en) * | 2014-05-30 | 2014-09-03 | 北京石大万嘉新材料科技有限公司 | Polymer microgel oil-displacing agent, preparing method thereof and applications thereof |
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2016
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104017131A (en) * | 2014-05-30 | 2014-09-03 | 北京石大万嘉新材料科技有限公司 | Polymer microgel oil-displacing agent, preparing method thereof and applications thereof |
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109422887B (en) * | 2017-08-22 | 2020-11-10 | 中国石油化工股份有限公司 | Anionic starch microsphere and preparation method and application thereof |
| CN109422887A (en) * | 2017-08-22 | 2019-03-05 | 中国石油化工股份有限公司 | A kind of anionic starch microballoon and its preparation method and application |
| CN109422886A (en) * | 2017-08-22 | 2019-03-05 | 中国石油化工股份有限公司 | A kind of anion doped spherex material and its preparation method and application |
| CN109422852A (en) * | 2017-08-22 | 2019-03-05 | 中国石油化工股份有限公司 | A kind of micron order spherex and its preparation method and application |
| CN109422851A (en) * | 2017-08-22 | 2019-03-05 | 中国石油化工股份有限公司 | A kind of cationic starch microballoon and its preparation method and application |
| CN109422886B (en) * | 2017-08-22 | 2020-11-06 | 中国石油化工股份有限公司 | Anion-doped starch microsphere material and preparation method and application thereof |
| WO2019037743A1 (en) * | 2017-08-22 | 2019-02-28 | 中国石油化工股份有限公司 | Starch-containing microsphere and preparation method therefor and application thereof |
| CN109422851B (en) * | 2017-08-22 | 2020-11-10 | 中国石油化工股份有限公司 | Cationic starch microsphere and preparation method and application thereof |
| CN109422852B (en) * | 2017-08-22 | 2021-01-26 | 中国石油化工股份有限公司 | Micron-sized starch microsphere and preparation method and application thereof |
| EP3670540A4 (en) * | 2017-08-22 | 2021-06-02 | China Petroleum & Chemical Corporation | Starch-containing microsphere and preparation method therefor and application thereof |
| US11891458B2 (en) | 2017-08-22 | 2024-02-06 | China Petroleum & Chemical Corporation | Starch-containing microsphere and preparation method and use thereof |
| CN112708011A (en) * | 2019-10-25 | 2021-04-27 | 中国石油化工股份有限公司 | Novel negative and positive composite flexible polymer microsphere and preparation method thereof |
| CN112708011B (en) * | 2019-10-25 | 2022-10-11 | 中国石油化工股份有限公司 | Novel negative and positive composite flexible polymer microsphere and preparation method thereof |
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Application publication date: 20170531 |