CN106590560A - Gel temporary plugging agent - Google Patents
Gel temporary plugging agent Download PDFInfo
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- CN106590560A CN106590560A CN201611104329.8A CN201611104329A CN106590560A CN 106590560 A CN106590560 A CN 106590560A CN 201611104329 A CN201611104329 A CN 201611104329A CN 106590560 A CN106590560 A CN 106590560A
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- Prior art keywords
- water
- gel
- agent
- glue
- temporary plugging
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- C—CHEMISTRY; METALLURGY
- 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
- C09K8/504—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
- C09K8/512—Compositions based on water or polar solvents containing organic compounds macromolecular compounds containing cross-linking agents
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- C—CHEMISTRY; METALLURGY
- 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
- C09K8/504—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
- C09K8/5083—Compositions based on water or polar solvents containing organic compounds macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
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- General Life Sciences & Earth Sciences (AREA)
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- Chemical Kinetics & Catalysis (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention discloses a gel temporary plugging agent. The gel temporary plugging agent is prepared from, by mass, 0.3-0.4% of partially hydrolyzed polyacrylamide, 0.03-0.08% of phenol crosslinking agent, 0.03-0.08% of aldehyde crosslinking agent, 0.05-0.2% of water soluble polyvinyl alcohol, 0.05-0.5% of hydrochloric acid or acetic acid, 0.2-0.5% of antioxidant and the balance water, and the sum of the mass percents of all the components is 100%, wherein the phenol crosslinking agent is one of combination of resorcinol and hydroquinone, the aldehyde crosslinking agent is urotropin, and the antioxidant is one or combination of diphenylamine, p-phenylenediamine and sodium fluoborate. The gelling time of the gel temporary plugging agent is adjustable in the range of 5-50 h, the gel breaking time is adjustable in the range of 120-240 h, after gel breaking, the viscosity is measured by a rotational viscometer at the shear rate of 70/s to be 5-10 mPa.s, which indicates thorough gel breakage, and therefore the gel temporary plugging agent can be suitable for most conventional oil deposit.
Description
Technical field：
The present invention relates to technical field of oilfield chemistry, more particularly to a kind of partially hydrolyzed polyacrylamide (PHPA) phenolic aldehyde frozen glue is temporarily blocked up
Agent.
Background technology：
With the continuous long period of development of water flood field, into after the mid-later development phase stage, there is comprehensive water cut rising, oil field
Exploitation benefit declines year by year.In order to improve recovery ratio, most oil wells all carried out fracturing reform, with oilfield exploitation not
Disconnected deeply the difficulty of stable high yield is increasing, and with the increase of the oil development time limit and measure number of times, the original people of old well
The production potential in work crack is less and less, and the single multiple fracturing technique such as extensive that adds can not meet oil field development volume increase surely
The development need of oil.Therefore, in order to improve oil well output, we can targetedly select the oil well of DEVELOPMENT PROSPECT to carry out two
Secondary or multiple fracturing reform is improving oily well yield.But during waterflooding extraction, injection water is always along old crack side
To water breakthrough, cause major part to carry out the old well moisture content that fracturing reform crosses and constantly rise.For the old well in this part, if still adopted
Carry out extending old crack with conventional refracturing method, it is difficult to reach the purpose for improving recovery ratio.Shown by field test：
Add diverting agent before pressing crack construction, block old crack, press off new crack, some oil wells after diverting agent construction, oil production
Greatly improve.Diverting agent is one of effective ways of old well volume increase.One of diverting agent the most frequently used at present is based on polymer
Agent, Organic substance is cross-linking agent, adds gel breaker.By the addition for controlling each component, kept for gelation time and broken glue time
In certain scope, diverting agent does not break glue during injection blocking agent, has noted the interior automatically broken glue of a period of time after blocking agent, so as to
Play the purpose of protection less permeable layer.However, presently used polymer high cost, it is big etc. that cross-linking agent there is also toxicity, zest
Shortcoming.The oxides such as gel breaker Ammonium persulfate. are added, complicated, poor operability is prepared.Therefore a kind of low cost is developed, letter is prepared
Single, safe frozen glue diverting agent is significant for old well increases production.
The content of the invention：
For the deficiencies in the prior art, it is an object of the invention to provide a kind of frozen glue diverting agent.
The purpose of the present invention is realized by following technical scheme：
The frozen glue diverting agent is made up of host, cross-linking agent, reinforcing agent, catalyst, antioxidant and water, and the host is portion
Divide hydrolyzed polyacrylamide, the cross-linking agent is phenolic crosslinkers, and the reinforcing agent is water-soluble poval, the catalysis
Agent is acid, and the antioxidant is reducing substanceses；The mass percent composition of each component is as follows:
Host 0.3%～0.4%, is partially hydrolyzed polyacrylamide (PHPA)；
Phenolic crosslinkers 0.03%～0.08%, are resorcinol or hydroquinone or its combination；
Aldehyde crosslinking agent 0.03%～0.08%, is hexamethylenamine；
Reinforcing agent 0.05%～0.2%, is water-soluble poval；
Catalyst 0.05%～0.5%, is hydrochloric acid or acetic acid or its combination；
Antioxidant 0.2%～0.5%, is one or a combination set of diphenylamines, p-phenylenediamine or Sodium fluoroborate；
Water, surplus；
The mass percent sum of each component is 100%.
According to currently preferred, the relative molecular mass of the partially hydrolyzed polyacrylamide (PHPA) is 1200 × 104~
1600×104, degree of hydrolysis 23%～28%；The water-soluble poval degree of polymerization is 1700～2400, and alcoholysis degree is 87%
～89%.
The preparation method of above-mentioned frozen glue diverting agent is as follows：
1st, in beaker partially hydrolyzed polyacrylamide (PHPA), water-soluble poval are filled in tap water by proportioning under room temperature
Divide dissolving, seal standby；Again by proportioning by cross-linking agent, reinforcing agent, catalyst, antioxidant and excess water mixing and stirring,
Sealing is standby.
2nd, above two solution mixing and stirring is obtained into plastic liquid.
3rd, take that 20ml is above-mentioned to be placed in 25ml ampoule bottles into glue, sealed with alcohol blast burner sintering, be placed in 40 DEG C～90 DEG C
Water-bath in heat 5～50h obtain final product frozen glue diverting agent of the present invention.
The invention has the beneficial effects as follows：
1st, partially hydrolyzed polyacrylamide (PHPA) used in the present invention is domestic general polymer, and low cost is easily obtained.Crosslinking
Agent is phenolic crosslinkers, and with hydroquinone, resorcinol phenol is substituted, and substitutes formaldehyde with hexamethylenamine, it is to avoid phenolic aldehyde
Toxicity and zest, improve safety.Contain hydroxyl in water-soluble poval simultaneously, can send out with phenolic cross-linking system
Raw reaction, with partially hydrolyzed polyacrylamide (PHPA) compound crosslinking system is collectively forming, and gel strength is improve, while height can be extended
The broken glue time under the conditions of temperature.
2nd, acid condition contributes to hexamethylenamine decomposition release formaldehyde, therefore adds hydrochloric acid or acetic acid, can be in low temperature bar
Promote the carrying out of cross-linking reaction under part, while excess H+Presence affect cross-linking reaction after amide structure stability, destruction freeze
The three-dimensional-structure of glue, makes frozen glue dehydration, broken glue.So can by adjust acid consumption to control gelation time and broken glue when
Between.In the range of 0.05%～0.5%, with the raising of sour consumption, gelation time shortens the consumption of acid, and the broken glue time also becomes
It is short.Under the conditions of 60 DEG C, when the consumption of acid is 0.2%, gelation time is 24h, and 100h starts brokenly glue, and 240h breaks completely glue, makes
With rotating cylinder viscometer in 70s-1Viscosity is determined under shear rate and is reduced to 5mPas～10mPas, wound is hardly brought to stratum
Evil.
3rd, frozen glue diverting agent of the present invention in Warning Blender agitators with 2000r/min high-speed stirred
After 5min, under 40 DEG C～90 DEG C temperature conditionss still can plastic, range estimation gel strength reach H ranks, resistant to shearing is functional.Together
When under the conditions of high temperature (90 DEG C) add antioxidant the Quick Oxidation under polymer high temperature can be suppressed degrade, control break glue when
Between.This frozen glue diverting agent gelation time is adjustable in 5h～50h, and the broken glue time is adjustable in 120h～240h, and gelling strength is high, breaks glue
Thoroughly, therefore, it is possible to being applied to most of routine oil reservoir.
Specific embodiment：
In order to be more clearly understood from the present invention, it is explained in detail in conjunction with embodiment, but the present invention protects model
Enclose and be not limited only to this.
Embodiment 1：
Add 0.05g resorcinol, 0.05g hexamethylenamine, 0.4g acetic acid, plus tap water to 50g in beaker, stirring is equal
It is even so as to fully dissolving, 0.3g partially hydrolyzed polyacrylamide (PHPA)s and 0.05g water-soluble povals are added in another beaker, then
Plus tap water fully dissolves to 50g, then the solution in above-mentioned two beaker is mixed, stirred, that is, obtain institute of the present invention
The frozen glue diverting agent stated is into glue.Take 20ml to be fitted in ampoule bottle, sintering sealing, when being placed in observation plastic in 45 DEG C of waters bath with thermostatic control
Between be 36h, break the glue time be 216h, after breaking gel viscosity be 7.8mPas.
Shut-off capacity is investigated：
Investigate the shut-off capacity of frozen glue provided by the present invention.Specific experiment process is as follows：It is 2.5cm, length by internal diameter
For 20cm two fill out sand tube filling quartz sand grain be obtained it is high and low ooze simulation core, 1# and 2# is denoted as, after water drive to pressure stability
Obtain original permeability k1, then by the above-mentioned inverse injection fill out sand tube into glue, injected slurry volume is 0.5PV (rock core pore-bodies
Product), it is then injected into 0.3PV water and is replaced, fill out sand tube is placed in 45 DEG C of waters bath with thermostatic control distinguishes aging 36h and 216h afterwards,
Water drive is finally distinguished to pressure stability, measure stifled rear permeability k of simulation core2, and by formula E=(k1-k2)/k1* 100%,
Reservoir core plugging rate E is calculated, experimental result is as shown in table 1：
The shut-off capacity of 1 embodiment of table 1 is tested
Embodiment 2：
0.06g resorcinol, 0.06g hexamethylenamine, 0.4g acetic acid, plus 5%NaCl aqueous solutions are added in beaker to 50g
Stir so as to fully dissolving, 0.3g partially hydrolyzed polyacrylamide (PHPA)s and 0.1g water-soluble polyethylenes are added in another beaker
Alcohol, then add 5%NaCl aqueous solutions fully to dissolve to 50g, then the solution in above-mentioned two beaker is mixed, stir, i.e.,
The frozen glue diverting agent of the present invention is obtained into glue.Take 20ml to be fitted in ampoule bottle, sintering sealing is placed in 45 DEG C of waters bath with thermostatic control and sees
It is 30h to examine gelation time, breaks the glue time for 200h, and after breaking gel viscosity is 7.3mPas.
Investigate the shut-off capacity of frozen glue provided by the present invention.Specific experiment process is as follows：It is 2.5cm, length by internal diameter
For 20cm two fill out sand tube filling quartz sand grain be obtained it is high and low ooze simulation core, 3# and 4# is denoted as, after water drive to pressure stability
Obtain original permeability k1, then by the above-mentioned inverse injection fill out sand tube into glue, injected slurry volume is 0.5PV (rock core pore-bodies
Product), it is then injected into 0.3PV water and is replaced, fill out sand tube is placed in 45 DEG C of waters bath with thermostatic control distinguishes aging 30h and 200h afterwards,
Water drive is finally distinguished to pressure stability, measure stifled rear permeability k of simulation core2, and by formula E=(k1-k2)/k1* 100%,
Reservoir core plugging rate E is calculated, experimental result is as shown in table 2：
The shut-off capacity of 2 embodiment of table 2 is tested
Embodiment 3：
Addition 0.06g resorcinol, 0.06g hexamethylenamine, 0.3g acetic acid, 0.2g Sodium fluoroborates in beaker, plus originally
Water stirs to 50g so as to fully dissolving, adds 0.35g partially hydrolyzed polyacrylamide (PHPA)s and 0.1g water-soluble in another beaker
Property polyvinyl alcohol, then add tap water fully dissolve to 50g, then by above-mentioned two beaker solution mix, stir, i.e.,
The frozen glue diverting agent of the present invention is obtained into glue.Take 20ml to be fitted in ampoule bottle, sintering sealing is placed in 65 DEG C of waters bath with thermostatic control and sees
It is 24h to examine gelation time, breaks the glue time for 192h, and after breaking gel viscosity is 6.5mPas.
Shut-off capacity is investigated：
Investigate the shut-off capacity of frozen glue provided by the present invention.Specific experiment process is as follows：It is 2.5cm, length by internal diameter
For 20cm two fill out sand tube filling quartz sand grain be obtained it is high and low ooze simulation core, 5# and 6# is denoted as, after water drive to pressure stability
Obtain original permeability k1, then by the above-mentioned inverse injection fill out sand tube into glue, injected slurry volume is 0.5PV (rock core pore-bodies
Product), it is then injected into 0.3PV water and is replaced, fill out sand tube is placed in 65 DEG C of waters bath with thermostatic control distinguishes aging 24h and 192h afterwards,
Water drive is finally distinguished to pressure stability, measure stifled rear permeability k of simulation core2, and by formula E=(k1-k2)/k1* 100%,
Reservoir core plugging rate E is calculated, experimental result is as shown in table 3：
The shut-off capacity of 3 embodiment of table 3 is tested
Embodiment 4：
0.06g resorcinol, 0.06g hexamethylenamine, 0.3g acetic acid, 0.3g Sodium fluoroborates are added in beaker of water, plus 5%
NaCl aqueous solutions stir to 50g so as to fully dissolving, add in another beaker 0.4g partially hydrolyzed polyacrylamide (PHPA)s and
0.1g water-soluble povals, then add 5%NaCl aqueous solutions fully to dissolve to 50g, then by the solution in above-mentioned two beaker
Mixing, stirs, that is, obtain the frozen glue diverting agent of the present invention into glue.Take 20ml to be fitted in ampoule bottle, sintering sealing is placed in
It is 20h that gelation time is observed in 65 DEG C of waters bath with thermostatic control, breaks the glue time for 160h, and after breaking gel viscosity is 6.4mPas.
Shut-off capacity is investigated：
Investigate the shut-off capacity of frozen glue provided by the present invention.Specific experiment process is as follows：It is 2.5cm, length by internal diameter
For 20cm two fill out sand tube filling quartz sand grain be obtained it is high and low ooze simulation core, 7# and 8# is denoted as, after water drive to pressure stability
Obtain original permeability k1, then by the above-mentioned inverse injection fill out sand tube into glue, injected slurry volume is 0.5PV (rock core pore-bodies
Product), it is then injected into 0.3PV water and is replaced, fill out sand tube is placed in 65 DEG C of waters bath with thermostatic control distinguishes aging 20h and 160h most afterwards
Water drive is distinguished afterwards to pressure stability, measures stifled rear permeability k of simulation core2, and by formula E=(k1-k2)/k1* 100%, meter
Reservoir core plugging rate E is calculated, experimental result is as shown in table 4：
The shut-off capacity of 4 embodiment of table 4 is tested
Embodiment 5：
0.08g resorcinol, 0.03g hydroquinone, 0.08g hexamethylenamine, 0.2g acetic acid, 0.3g fluorine are added in beaker
Sodium borate, 0.2g diphenylamines, plus 5%NaCl aqueous solutions stir to 50g so as to fully dissolving, add in another beaker
0.4g partially hydrolyzed polyacrylamide (PHPA)s and 0.15g water-soluble povals, then add 5%NaCl aqueous solutions fully to dissolve to 50g, so
The solution in above-mentioned two beaker is mixed afterwards, is stirred, that is, obtain the frozen glue diverting agent of the present invention into glue.Take 20ml dresses
In entering ampoule bottle, sintering sealing, it is 18h to be placed in 85 DEG C of waters bath with thermostatic control and observe gelation time, and the broken glue time is 144h, after breaking gel
Viscosity is 5.2mPas.
Shut-off capacity is investigated：
Investigate the shut-off capacity of frozen glue provided by the present invention.Specific experiment process is as follows：It is 2.5cm, length by internal diameter
For 20cm two fill out sand tube filling quartz sand grain be obtained it is high and low ooze simulation core, be denoted as 9# and 10#, water drive is to pressure stability
After obtain original permeability k1, then by the above-mentioned inverse injection fill out sand tube into glue, injected slurry volume is 0.5PV (rock core holes
Volume), be then injected into 0.3PV water and replaced, afterwards by fill out sand tube be placed in 85 DEG C of waters bath with thermostatic control distinguish aging 18h and
144h, finally respectively water drive, to pressure stability, measures stifled rear permeability k of simulation core2, and by formula E=(k1-k2)/k1*
100%, reservoir core plugging rate E is calculated, experimental result is as shown in table 5：
The shut-off capacity of 5 embodiment of table 5 is tested
Embodiment 6：
0.08g resorcinol, 0.05g hydroquinone, 0.08g hexamethylenamine, 0.2g acetic acid, 0.4g fluorine are added in beaker
Sodium borate, 0.4g diphenylamines, plus 5%NaCl+0.1%CaCl2+ 0.1%MgCl2Aqueous solution to 50g stirs so as to fully
Dissolving, adds 0.4g partially hydrolyzed polyacrylamide (PHPA)s and 0.2g water-soluble povals in another beaker, add by 5%NaCl
+ 0.1%CaCl2+ 0.1%MgCl2The mixed aqueous solution of composition fully dissolves to 50g, then by the solution in above-mentioned two beaker
Mixing, stirs, that is, obtain the frozen glue diverting agent of the present invention into glue.Take 20ml to be fitted in ampoule bottle, sintering sealing is placed in
It is 7h that gelation time is observed in 85 DEG C of waters bath with thermostatic control, breaks the glue time for 120h, and after breaking gel viscosity is 5.0mPas.
Shut-off capacity is investigated：
Investigate the shut-off capacity of frozen glue provided by the present invention.Specific experiment process is as follows：It is 2.5cm, length by internal diameter
For 20cm two fill out sand tube filling quartz sand grain be obtained it is high and low ooze simulation core, be denoted as 11# and 12#, water drive is to pressure stability
After obtain original permeability k1, then by the above-mentioned inverse injection fill out sand tube into glue, injected slurry volume is 0.5PV (rock core holes
Volume), it is then injected into 0.3PV water and is replaced, fill out sand tube is placed in 85 DEG C of waters bath with thermostatic control distinguishes aging 7h and 120h afterwards,
Water drive is finally distinguished to pressure stability, measure stifled rear permeability k of simulation core2, and by formula E=(k1-k2)/k1* 100%,
Reservoir core plugging rate E is calculated, experimental result is as shown in table 6：
The shut-off capacity of 6 embodiment of table 6 is tested
Table 1 to table 6 test result indicate that：The diverting agent that the present invention is provided has excellent sealing characteristics, and low permeability cores exist
Sealing ratiod is more than 99% after frozen glue plastic；Hypertonic rock core after frozen glue plastic sealing ratiod more than 97%；High low permeability cores exist
Sealing ratiod is below 10% after Gel Breakdown.So this diverting agent can effectively block during water drive crude oil occur it is hypertonic
Layer, is conducive to the raising of oil recovery factor；After breaking gel, sealing ratiod becomes very low, minimum to formation damage.
Claims (3)
1. a kind of frozen glue diverting agent, it is characterised in that its component and its mass percent composition are as follows：Partial hydrolysiss polyacrylamide
Amine 0.3%～0.4%, Phenolic crosslinkers 0.03%～0.08%, aldehyde crosslinking agent 0.03%～0.08%, water-soluble polyethylene
Alcohol 0.05%～0.20%, catalyst 0.05%～0.50%, antioxidant 0.2%～0.5%, balance of water, the matter of each component
Amount percentage ratio sum is 100%；Wherein described Phenolic crosslinkers are resorcinol or hydroquinone or its combination；Aldehydes is crosslinked
Agent is hexamethylenamine；Catalyst is acetic acid or hydrochloric acid or its combination；Antioxidant be diphenylamines or p-phenylenediamine or Sodium fluoroborate or
Its combination.
2. frozen glue diverting agent according to claim 1, it is characterised in that described partially hydrolyzed polyacrylamide (PHPA) it is relative
Molecular mass is 1200 × 104～1600 × 104, degree of hydrolysis is 23%～28%.
3. frozen glue diverting agent according to claim 1, it is characterised in that the degree of polymerization of described water-soluble poval is
1700～2400, alcoholysis degree is 87%～89%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611104329.8A CN106590560A (en) | 2016-12-05 | 2016-12-05 | Gel temporary plugging agent |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611104329.8A CN106590560A (en) | 2016-12-05 | 2016-12-05 | Gel temporary plugging agent |
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| CN106590560A true CN106590560A (en) | 2017-04-26 |
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| CN201611104329.8A Pending CN106590560A (en) | 2016-12-05 | 2016-12-05 | Gel temporary plugging agent |
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Cited By (5)
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| CN111087999A (en) * | 2020-01-10 | 2020-05-01 | 任丘市油联化工有限公司 | High-temperature-resistant profile control agent for oil extraction and preparation method thereof |
| CN111574977A (en) * | 2020-05-29 | 2020-08-25 | 中国石油大学(华东) | Medium-high temperature oil reservoir phenolic gel self-degradation temporary plugging agent and preparation method thereof |
| CN113234426A (en) * | 2021-04-30 | 2021-08-10 | 河北科技大学 | Reversible composite gel, preparation method and application |
| CN115449037A (en) * | 2022-08-08 | 2022-12-09 | 成都理工大学 | Modified polyalcohol drilling flushing fluid |
| CN116064010A (en) * | 2021-11-01 | 2023-05-05 | 中国石油化工股份有限公司 | Raw material composition of high-temperature-resistant high-salt plugging agent, preparation method and application |
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| CN111574977A (en) * | 2020-05-29 | 2020-08-25 | 中国石油大学(华东) | Medium-high temperature oil reservoir phenolic gel self-degradation temporary plugging agent and preparation method thereof |
| CN113234426A (en) * | 2021-04-30 | 2021-08-10 | 河北科技大学 | Reversible composite gel, preparation method and application |
| CN116064010A (en) * | 2021-11-01 | 2023-05-05 | 中国石油化工股份有限公司 | Raw material composition of high-temperature-resistant high-salt plugging agent, preparation method and application |
| CN116064010B (en) * | 2021-11-01 | 2024-06-04 | 中国石油化工股份有限公司 | Raw material composition of high-temperature-resistant high-salt plugging agent, preparation method and application |
| CN115449037A (en) * | 2022-08-08 | 2022-12-09 | 成都理工大学 | Modified polyalcohol drilling flushing fluid |
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