CN105114032B - A kind of method that use cross-linked polymer gel sealing agent carries out middle-deep well leak stopping - Google Patents
A kind of method that use cross-linked polymer gel sealing agent carries out middle-deep well leak stopping Download PDFInfo
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Abstract
The present invention relates to a kind of method that use cross-linked polymer gel sealing agent carries out middle-deep well leak stopping, raw material weight ratio is purified cotton sodium salt solution：120 parts, acrylamide：75~85 parts, ammonium persulfate：13~17 parts, cerous sulfate：2~5 parts, β D mannuronic acids（M）：4 parts, ammonium dihydrogen phosphate：1~1.5 part, composite Portland cement slurry：100 parts and mix type microfibre：150~200 parts；The ratio of mud of composite Portland cement slurry is 0.44；Acrylamide, ammonium persulfate particle, cerous sulfate particle, β D mannuronic acids are added into purified cotton sodium salt solution successively（M）, composite Portland cement slurry, mix type microfibre and ammonium dihydrogen phosphate stirs evenly and obtains sealing agent；Then sealing agent is delivered into drop ply, for pressure testing after slurry in drilling rod, if bottom pressure rises, standing carries out well for slurry after building the pressure, then stands and build the pressure 12 hours, carried out leak stopping pressure-bearing test, when being pumped normal, proceed operation of drilling.This method leak stopping is reliable and high temperature resistance resistance to compression.
Description
Technical field
The present invention relates to a kind of method that use cross-linked polymer gel sealing agent carries out middle-deep well leak stopping, belong to petroleum drilling
Well technical field.
Background technology
Leakage is the technical barrier frequently encountered in drilling process, and especially high temperature leakage can cause a large amount of streams of drilling fluid
Lose, cause the rising of drilling cost, while bottom pressure can be caused to change, induce borehole well instability, well slough, well kick, blowout
Etc. the generation of complex accident, the raising of bit speed seriously govern.
It is general to use due to lacking the leakage stopping technology of high temperature resistance at present when oil drilling bores and meets high-temperature stratum leakage section
Conventional sealing agent leak stopping.Country's processing high temperature leakage generally uses bridge joint leak stopping, and bridge joint leak stopping has economy, user
Just, the advantage of construction safety, can solve the partial loss that is caused by hole and crack and leakage is returned in mistake.The bridge joint that the country is used
Loss circulation material is roughly divided into three classes：Hard fruit shell class, fibrous material and lamellar material.It is any kind in Process of Leaking Stoppage
Material is used alone, and it is all limited that it, which is acted on, above-mentioned three classes material only is matched somebody with somebody into compound use with rational ratio and level,
Due effect can be received, but deepening continuously with drilling, the temperature on leakage stratum is also constantly being raised, and is immersed in mud
In hard fruit shell class material and plant fiber material such as walnut shell, hazelnut shell, cotton seed hulls and sawdust etc., in well high temperature,
Under conditions of high pressure and alkali corrosion, over time, these materials will slowly soften, corrode, or even some material meetings
Burnt, cause bridge joint intensity drastically to decline, it is easy to cause leak stopping failure or secondary leakage, it is impossible to fundamentally solve high temperature
The problem of leak stopping.
Well depth is that 4000~5000m is referred to as middle-deep well, and downhole temperature is generally at 120 DEG C~140 DEG C.Though conventional blocking method
Effect so has been played for the stoppage engineering of oil drilling, but there is shortcoming or deficiency simultaneously, high-temperature resistance is low, the term of validity
Short, leak stopping inefficient, loss circulation material consumption are big, plugging time length, poor in high temperature deep well and geothermal well leak stopping safety coefficient, easily
There is down hole problem, these shortcomings directly affect the probing development process of high temperature well and geothermal well, therefore traditional high temperature
Loss circulation material far from disclosure satisfy that the leak stopping demand of growing deep-well Holes of Complicated Wells, therefore study a kind of high temperature deep well
It is very necessary with high temperature resistance sealing agent.
The content of the invention
It is an object of the present invention to overcome problems of the prior art to use cross-linked polymer gel there is provided one kind
The method that sealing agent carries out middle-deep well leak stopping, leak stopping is reliable, and high temperature resistance, anti-pressure ability are strong.
To solve above technical problem, of the invention is a kind of using the progress middle-deep well leak stopping of cross-linked polymer gel sealing agent
Method, in turn include the following steps：(1) raw material, purified cotton sodium salt solution are prepared by following components and weight content：120 parts,
Acrylamide：（75~85）Part, ammonium persulfate：（13~17）Part, cerous sulfate：（2~5）Part, beta-D-mannuronic acid（M）：4
Part, ammonium dihydrogen phosphate：（1~1.5）Part, composite Portland cement slurry：100 parts and mix type microfibre：（150~200）Part；Institute
The ratio of mud for stating composite Portland cement slurry is 0.44；(2) acrylamide is added into purified cotton sodium salt solution, with 400r/min
Rotating speed carry out high-speed stirred and be sufficiently mixed both in 10 minutes, moderate-speed mixer, middling speed are then carried out with 300r/min rotating speed
60 DEG C are heated to while stirring and constant temperature is kept；(3) nitrogen is continually fed into step reaction product (2) and reaction vessel,
Nitrogen is passed through to keep moderate-speed mixer and being maintained at 60 DEG C of constant temperature after 3 minutes, be slowly added to ammonium persulfate particle, reaction until
After particulate matter disappears, continue back flow reaction 1.5 hours；(4) temperature is increased to 80 DEG C and keeps constant temperature, keep moderate-speed mixer
Under, cerous sulfate particle is slowly added to, the charge door of reaction vessel is then shut off, the charge of nitrogen is lifted, reaction vessel is kept
Interior pressure is 1.3MPa, back flow reaction more than 3 hours until reactant presentation white emulsion shape, obtains cross-linked polymer and coagulate
Glue；Detect the molecular weight of the cross-linked polymer gel more than 4,000,000；(5) in the state of moderate-speed mixer is kept, to above-mentioned
Beta-D-mannuronic acid is slowly added in cross-linked polymer gel（M）, addition continues moderate-speed mixer 10 minutes after finishing, and adjusts
PH value is 7~7.5；(6) composite Portland cement slurry is added into step reaction product (5) and mixes type microfibre, middling speed is stirred
Mix more than 15 minutes until well mixed；(7) ammonium dihydrogen phosphate added into step reaction product (6), moderate-speed mixer 10 minutes,
Obtain middle-deep well cross-linked polymer gel sealing agent；(8) continue moderate-speed mixer after 10 minutes, start drilling fluid pump by above-mentioned middle depth
Well cross-linked polymer gel sealing agent is through Drill-pipe conveyed to drop ply, and the discharge capacity of drilling fluid pump is 1.5m3/min, and continuous conveying 60
~90m3；(9) continue to convey drilling fluid into drilling rod using drilling fluid pump, until the middle-deep well cross-linked polymer in drilling rod is coagulated
Glue sealing agent all replaces with drilling fluid, is then shut off drilling fluid pump and carries out standing building the pressure leak stopping 60 minutes；(10) brill is reopened
Well liquid pump carries out pressure testing, if not occurring bottom pressure rising after pressure testing, and repeat step is (1) to (9) after closing drilling fluid pump；(11) try
If occurring bottom pressure rising after pressure, close drilling fluid pump continuation standing and build the pressure 20 minutes, be then again started up drilling fluid pump,
And control the discharge capacity of drilling fluid pump for 0.2~0.3m3/min, the middle-deep well cross-linked polymer gel between well and drilling rod is blocked up
Leakage agent all replace with drilling fluid, when after drilling fluid is returned out from well head close drilling fluid pump proceed standing build the pressure 12 it is small when；
Standing build the pressure 12 hours during every 30 minutes, to underground supplement a drilling fluid, return out stopping from well head again to drilling fluid；
Open drilling fluid pump carry out leak stopping pressure-bearing test, when the pump pressure of drilling fluid pump return to miss before normal value when, continue into
Capable operation of drilling.
Relative to prior art, the present invention achieves following beneficial effect：1. purified cotton sodium salt provides the fibre of cross-linking reaction
Dimension element, acrylamide plays bridge formation suction-operated, cellulose is flocculated, is cross-linked with each other.Ammonium persulfate triggers cross-linking reaction,
Make fiber destarch simultaneously；Nitrogen is passed through before ammonium persulfate is added, it is ensured that reaction environment anaerobic, it is to avoid cellulose is in cross-linking process
In rise viscous, influence the molecular weight of final cross-linking products；Back flow reaction 1.5h is ensured in the presence of cross-linking reaction initiator, is refined
Gossypin and can provide bridge formation suction-operated acrylamide is full cross-linked, copolyreaction, make cellulose molecular chain elongated, and
Molecular weight increases severely.Cerous sulfate further triggers between cellulose and acrylamide, cellulose and acrylamide pass through ammonium persulfate
Mutually it is grafted between copolymerzation with cross-linking reaction product and between cellulose and copolymerzation with cross-linking reactant, makes the high molecular polymer of generation
Molecular weight it is bigger, strand has more side chains, for after formation in the presence of thixotropic agent formed gel provide more
Side chain, the gel strength of formation is higher.Reaction mechanism is：
。
2. the molecular weight of cross-linked polymer gel 4,000,000 crosslinkings described above, copolymerization, graft reaction very fully, be shape
Intensity into " block wall " provides guarantee.3. beta-D-mannuronic acid is added in cross-linked polymer gel（M）Afterwards, β-D-MANNOSE
Aldehydic acid（M）Sodium ion exchanged with the amide groups in cross-linked polymer gel, carboxyl position carry out ionic compartmentation, so as to occur
Gelling reaction, forms blob of viscose.Beta-D-mannuronic acid（M）When pH is reduced, viscosity can increase, and there is viscosity when pH is 6.7 and touch
Become, with certain alkali resistance, when pH is 7~7.5, the blob of viscose of formation has more preferable shear thinning behavior, is provided with for pumping
Sharp condition.4. composite Portland cement slurry can provide the intensity and anti-pressure ability of blob of viscose；After cross-linked polymer gel gelling, such as
Fruit is without enough bridge particles, and the blob of viscose intensity of formation is only capable of reaching 1~2MPa, it is impossible to which the pressure-bearing for meeting middle-deep well is blocked up
Leakage is required；Bridge particle can be played a part of by mixing type microfibre, and phase has been cross-linked to form with natural fiber using synthetic fibers
The net high-polymer polymer mutually wound, high molecular polymerization frozen glue slowly starts gelling, complete gelation under the high-temperature condition of underground
Afterwards, the intensity for forming blob of viscose can reach 15MPa, can resist more than 140 DEG C of high temperature, can meet 4000~5000m's of well depth
The leak stopping of middle-deep well needs.Mix the adding proportion of type microfibre in the present invention so that sealing agent has highest intensity, if
Continue to improve the weight ratio for mixing type microfibre, the chemical crosslinking of gel chemistries material can be disturbed to act on the contrary, can be reduced on the contrary
The bearing capacity of its leak stopping.5. the ammonium dihydrogen phosphate of ratio of the present invention is added, can be by gelling control in suitable time range
It is interior, both ensured before gelling, sealing agent can be pumped to drop ply, drilling rod and replacing in well can be completed before gelling again
Slurry, additionally it is possible to make sealing agent be gelled in time after reaching drop ply so that leak stopping slurries stop to live in drop ply.6. sealing agent is pumped
Shi Caiyong discharge capacities are 1.5m3/min, have both avoided discharge capacity is excessive from causing the formation fracture for having occurred and that leakage to enter one under huge discharge
Step expands, and sealing agent can all make a gift to someone drop ply before initial set again；For the situation of most of small leakages and middle leakage, with reference to gelling
Leak stopping plays the glue time, 60~90m3 is conveyed every time the most appropriate.7. after sealing agent conveying drop ply, drilling rod is first completed using drilling fluid
In for slurry, built the pressure subsequently into standing, prevent cross-linked polymer gel to be gelled in drilling rod, blocking drilling rod centre bore
Road.8. pressure testing does not show bottom pressure and risen, and illustrates leak stopping failure, it is necessary to carry out leak stopping again；Occur after pressure testing on bottom pressure
Rise, illustrate that leak stopping success builds the pressure 20 minutes, it is necessary to stand, after the 1~2MPa of rising for making drop ply blob of viscose intensity, then complete well
For slurry, prevent well by drilling rod locking, the displacement control of drilling fluid pump prevents discharge capacity excessive to drop ply in 0.2~0.3m3/min
Newly formed blob of viscose formation is impacted and broken, has adverse effect on, causes leak stopping to fail.9. after the completion of well is for slurry, continue
Standing is built the pressure 12 hours, waits blob of viscose to reach predetermined intensity, then carries out pressure-bearing experiment, and the pump pressure of drilling fluid pump is returned to Lou
During normal value before mistake, illustrate that leak stopping is completely successful, can proceed with operation of drilling.
As the present invention preferred scheme, step (1) in raw material components and weight content it is as follows, purified cotton sodium salt solution：
120 parts, acrylamide：75 parts, ammonium persulfate：13 parts, cerous sulfate：2 parts, beta-D-mannuronic acid（M）：4 parts, biphosphate
Ammonium：1 part, composite Portland cement slurry：100 parts and mix type microfibre：150 parts.
As the present invention preferred scheme, step (1) in raw material components and weight content it is as follows, purified cotton sodium salt solution：
120 parts, acrylamide：80 parts, ammonium persulfate：15 parts, cerous sulfate：3 parts, beta-D-mannuronic acid（M）：4 parts, biphosphate
Ammonium：1.2 parts, composite Portland cement slurry：100 parts and mix type microfibre：180 parts.
As the present invention preferred scheme, step (1) in raw material components and weight content it is as follows, purified cotton sodium salt solution：
120 parts, acrylamide：85 parts, ammonium persulfate：17 parts, cerous sulfate：5 parts, beta-D-mannuronic acid（M）：4 parts, biphosphate
Ammonium：1.5 parts, composite Portland cement slurry：100 parts and mix type microfibre：200 parts.
As the preferred scheme of the present invention, the preparation method of the purified cotton sodium salt is as follows：1. the cotton fiber degree of polymerization is prepared
The sodium hydroxide solution that purified cotton and concentration expressed in percentage by weight for 12000~14000 are 17.5~18%, purified cotton and hydroxide
The weight ratio of sodium solution is 5:2；2. will purified cotton put into sodium hydroxide solution in, stirred at 60 DEG C and react 1.5 hours with
On, until uniform white suspension emulsion is presented, obtain purified cotton sodium salt just solution；3. solution at the beginning of purified cotton sodium salt is surpassed
Sound micro-vibration 30 minutes, obtains purified cotton sodium salt solution, and supersonic frequency is 20kHz~30kHz, and ultrasonication intensity is 2.0 W/
Cm2~3.0W/cm2.Purified cotton and sodium hydroxide reaction generation purified cotton sodium salt so that being sufficiently humidified so as to inside purified cotton
Expansion, improves the reactivity of purified cotton, is conducive to further cross-linking reaction.It is ultrasonically treated to improve purified cotton sodium salt
Molecule link Zhi Chengdu, more meet Zhi Duan subsequently to be provided with crosslinking agent.Reaction mechanism is：
。
As the preferred scheme of the present invention, the type microfibre that mixes is carried out uniformly by calcium carbonate crystal whisker and organic microfiber
Mix and form, the mixing ratio of the calcium carbonate crystal whisker and organic microfiber is 0.8:1.Calcium carbonate crystal whisker and organic microfiber are uniform
It is dispersed in cross-linked polymer gel, mutually wind netted is cross-linked to form with the high molecular polymer in cross-linked polymer gel
High molecular polymer.Calcium carbonate crystal whisker is to form " block wall " to provide physical supporting role, and its intensity is substantially improved；Have
Machine microfibre is mutually wound with calcium carbonate crystal whisker, is provided physical supporting role for " block wall " of formation, is made its intensity big
Width is lifted；Meanwhile, add the intensity of " block wall " when being deformed under being acted on by strata pressure.
As preferred scheme of the invention further, 20~30 μm of the length of the calcium carbonate crystal whisker, 0.5~1 μm of diameter,
PH value 9.0~9.5, modulus of elasticity is 410~710GPa and tensile strength is not less than 2.058GPa；The organic microfiber is by gathering
The weight of ester fiber and polypropylene fibre composition, polyester fiber and polypropylene fibre is 7:3；The diameter 20 of the polyester fiber~
25 μm, 6~9mm of length, elongation at break >=15%, tensile strength >=960MPa and modulus of elasticity >=9000MPa；Described poly- third
The length of alkene fiber is 10~20mm, filament number≤2.2dtex, tensile strength >=660MPa, modulus of elasticity >=350MPa.It is poly-
Tacryl can improve the intensity of " block wall ", improve the rebound performance of " block wall " after compressive deformation.Polyester fiber can change
Anti-fatigue performance, cracking resistance and the high temperature stability performance of kind " block wall ", can effectively improve the tension of " block wall ", resistance to compression,
Anti-shearing and impact strength, makes up deficiency of the polypropylene fibre at heat-resisting and ageing-resistant aspect.
As further preferred scheme of the invention, the polyester fiber and polypropylene fibre are at 60 DEG C hydrophilic whole
Manage in agent and soak 3 hours.Due to polyester fiber and polypropylene fibre compound with regular structure but hydrophily is poor, in cross-linked polymer gel
It is difficult to be uniformly dispersed, surface modification treatment is carried out using hydrophilic finishing agent to polyester fiber and polypropylene fibre, its parent can be improved
Aqueous energy, is conducive to them dispersed in polymer gel, makes " block wall " structure and the even intensity to be formed.
Embodiment
Embodiment one
The method that a kind of use cross-linked polymer gel sealing agent of the present invention carries out middle-deep well leak stopping, successively including as follows
Step：
(1) following components and weight content prepare raw material, purified cotton sodium salt solution：120 parts, acrylamide：75 parts, over cure
Sour ammonium：13 parts, cerous sulfate：2 parts, beta-D-mannuronic acid（M）：4 parts, ammonium dihydrogen phosphate：1 part, composite Portland cement slurry：
100 parts and mix type microfibre：150 parts；The ratio of mud of the composite Portland cement slurry is 0.44；
(2) acrylamide is added in purified cotton sodium salt solution, carrying out high-speed stirred with 400r/min rotating speed makes two in 10 minutes
Person is sufficiently mixed, and then carries out moderate-speed mixer with 300r/min rotating speed, and 60 DEG C are heated to while moderate-speed mixer and keeps permanent
Temperature；
(3) nitrogen is continually fed into step reaction product (2) and reaction vessel, is passed through nitrogen after 3 minutes in holding
Speed is stirred and is maintained at 60 DEG C of constant temperature, is slowly added to ammonium persulfate particle, reaction until after particulate matter disappearance, continuing backflow anti-
Answer 1.5 hours；
(4) temperature is increased to 80 DEG C and keeps constant temperature, in the case where keeping moderate-speed mixer, be slowly added to cerous sulfate particle, then
The charge door of reaction vessel is closed, the charge of nitrogen is lifted, it is 1.3MPa, back flow reaction 3 to keep the pressure in reaction vessel
Hour is until reactant presentation white emulsion shape, obtains cross-linked polymer gel；Detect the molecule of the cross-linked polymer gel
Amount is more than 4,000,000；
(5) in the state of moderate-speed mixer is kept, beta-D-mannuronic acid is slowly added into above-mentioned cross-linked polymer gel
（M）, addition continues moderate-speed mixer 10 minutes after finishing, and it is 7 to adjust pH value；
(6) composite Portland cement slurry is added into step reaction product (5) and mixes type microfibre, 15 points of moderate-speed mixer
More than clock until well mixed；
(7) ammonium dihydrogen phosphate is added into step reaction product (6), and moderate-speed mixer 10 minutes obtains middle-deep well crosslinking poly-
Compound GEL USED FOR PLUGGING WELL LOST CIRCULATION；
(8) continue moderate-speed mixer after 10 minutes, start drilling fluid pump and pass through above-mentioned middle-deep well cross-linked polymer gel sealing agent
Drill-pipe conveyed is to drop ply, and the discharge capacity of drilling fluid pump is 1.5m3/min, and continuous conveying 60m3；
(9) continue to convey drilling fluid into drilling rod using drilling fluid pump, until the middle-deep well cross-linked polymer in drilling rod is coagulated
Glue sealing agent all replaces with drilling fluid, is then shut off drilling fluid pump and carries out standing building the pressure leak stopping 60 minutes；
(10) reopen drilling fluid pump and carry out pressure testing, if not occurring bottom pressure rising after pressure testing, close drilling fluid pump
Repeat step is (1) to (9) afterwards；
If (11) occurring bottom pressure rising after pressure testing, close drilling fluid pump continuation standing and build the pressure 20 minutes, then again
Start drilling fluid pump, and control the discharge capacity of drilling fluid pump for 0.2m3/min, by the middle-deep well cross-linked polymeric between well and drilling rod
Thing GEL USED FOR PLUGGING WELL LOST CIRCULATION all replaces with drilling fluid, and drilling fluid pump is closed after drilling fluid is returned out from well head and proceeds standing and builds the pressure
12 hours；Standing build the pressure 12 hours during every 30 minutes, to underground supplement a drilling fluid, returned again from well head to drilling fluid
Go out to stop；
(12) open drilling fluid pump and carry out leak stopping pressure-bearing test, the normal value returned to when the pump pressure of drilling fluid pump before leakage
When, proceed operation of drilling.
Embodiment two
The method that a kind of use cross-linked polymer gel sealing agent of the present invention carries out middle-deep well leak stopping, successively including as follows
Step：
(1) following components and weight content prepare raw material, purified cotton sodium salt solution：120 parts, acrylamide：80 parts, over cure
Sour ammonium：15 parts, cerous sulfate：3 parts, beta-D-mannuronic acid（M）：4 parts, ammonium dihydrogen phosphate：1.2 parts, composite Portland cement slurry：
100 parts and mix type microfibre：180 parts；The ratio of mud of the composite Portland cement slurry is 0.44；
(2) acrylamide is added in purified cotton sodium salt solution, carrying out high-speed stirred with 400r/min rotating speed makes two in 10 minutes
Person is sufficiently mixed, and then carries out moderate-speed mixer with 300r/min rotating speed, and 60 DEG C are heated to while moderate-speed mixer and keeps permanent
Temperature；
(3) nitrogen is continually fed into step reaction product (2) and reaction vessel, is passed through nitrogen after 3 minutes in holding
Speed is stirred and is maintained at 60 DEG C of constant temperature, is slowly added to ammonium persulfate particle, reaction until after particulate matter disappearance, continuing backflow anti-
Answer 1.5 hours；
(4) temperature is increased to 80 DEG C and keeps constant temperature, in the case where keeping moderate-speed mixer, be slowly added to cerous sulfate particle, then
The charge door of reaction vessel is closed, the charge of nitrogen is lifted, it is 1.3MPa, back flow reaction to keep the pressure in reaction vessel
3.5 hours until reactant presentation white emulsion shape, obtains cross-linked polymer gel；Detect point of the cross-linked polymer gel
Son amount is more than 4,000,000；
(5) in the state of moderate-speed mixer is kept, beta-D-mannuronic acid is slowly added into above-mentioned cross-linked polymer gel
（M）, addition continues moderate-speed mixer 10 minutes after finishing, and it is 7.5 to adjust pH value；
(6) composite Portland cement slurry is added into step reaction product (5) and mixes type microfibre, 15 points of moderate-speed mixer
More than clock until well mixed；
(7) ammonium dihydrogen phosphate is added into step reaction product (6), and moderate-speed mixer 10 minutes obtains middle-deep well crosslinking poly-
Compound GEL USED FOR PLUGGING WELL LOST CIRCULATION；
(8) continue moderate-speed mixer after 10 minutes, start drilling fluid pump and pass through above-mentioned middle-deep well cross-linked polymer gel sealing agent
Drill-pipe conveyed is to drop ply, and the discharge capacity of drilling fluid pump is 1.5m3/min, and continuous conveying 70m3；
(9) continue to convey drilling fluid into drilling rod using drilling fluid pump, until the middle-deep well cross-linked polymer in drilling rod is coagulated
Glue sealing agent all replaces with drilling fluid, is then shut off drilling fluid pump and carries out standing building the pressure leak stopping 60 minutes；
(10) reopen drilling fluid pump and carry out pressure testing, if not occurring bottom pressure rising after pressure testing, close drilling fluid pump
Repeat step is (1) to (9) afterwards；
If (11) occurring bottom pressure rising after pressure testing, close drilling fluid pump continuation standing and build the pressure 20 minutes, then again
Start drilling fluid pump, and control the discharge capacity of drilling fluid pump for 0.25m3/min, the middle-deep well between well and drilling rod is crosslinked poly-
Compound GEL USED FOR PLUGGING WELL LOST CIRCULATION all replaces with drilling fluid, and drilling fluid pump is closed after drilling fluid is returned out from well head and proceeds standing and suppresses
Pressure 12 hours；Standing build the pressure 12 hours during every 30 minutes, to underground supplement a drilling fluid, to drilling fluid again from well head
Return out stopping；
(12) open drilling fluid pump and carry out leak stopping pressure-bearing test, the normal value returned to when the pump pressure of drilling fluid pump before leakage
When, proceed operation of drilling.
Embodiment three
The method that a kind of use cross-linked polymer gel sealing agent of the present invention carries out middle-deep well leak stopping, successively including as follows
Step：
(1) following components and weight content prepare raw material, purified cotton sodium salt solution：120 parts, acrylamide：85 parts, over cure
Sour ammonium：17 parts, cerous sulfate：5 parts, beta-D-mannuronic acid（M）：4 parts, ammonium dihydrogen phosphate：1.5 parts, composite Portland cement slurry：
100 parts and mix type microfibre：200 parts；The ratio of mud of the composite Portland cement slurry is 0.44；
(2) acrylamide is added in purified cotton sodium salt solution, carrying out high-speed stirred with 400r/min rotating speed makes two in 10 minutes
Person is sufficiently mixed, and then carries out moderate-speed mixer with 300r/min rotating speed, and 60 DEG C are heated to while moderate-speed mixer and keeps permanent
Temperature；
(3) nitrogen is continually fed into step reaction product (2) and reaction vessel, is passed through nitrogen after 3 minutes in holding
Speed is stirred and is maintained at 60 DEG C of constant temperature, is slowly added to ammonium persulfate particle, reaction until after particulate matter disappearance, continuing backflow anti-
Answer 1.5 hours；
(4) temperature is increased to 80 DEG C and keeps constant temperature, in the case where keeping moderate-speed mixer, be slowly added to cerous sulfate particle, then
The charge door of reaction vessel is closed, the charge of nitrogen is lifted, it is 1.3MPa, back flow reaction to keep the pressure in reaction vessel
3.5 hours until reactant presentation white emulsion shape, obtains cross-linked polymer gel；Detect point of the cross-linked polymer gel
Son amount is more than 4,000,000；
(5) in the state of moderate-speed mixer is kept, beta-D-mannuronic acid is slowly added into above-mentioned cross-linked polymer gel
（M）, addition continues moderate-speed mixer 10 minutes after finishing, and adjusts pH value 7.5；
(6) composite Portland cement slurry is added into step reaction product (5) and mixes type microfibre, 15 points of moderate-speed mixer
More than clock until well mixed；
(7) ammonium dihydrogen phosphate is added into step reaction product (6), and moderate-speed mixer 10 minutes obtains middle-deep well crosslinking poly-
Compound GEL USED FOR PLUGGING WELL LOST CIRCULATION；
(8) continue moderate-speed mixer after 10 minutes, start drilling fluid pump and pass through above-mentioned middle-deep well cross-linked polymer gel sealing agent
Drill-pipe conveyed is to drop ply, and the discharge capacity of drilling fluid pump is 1.5m3/min, and continuous conveying 90m3；
(9) continue to convey drilling fluid into drilling rod using drilling fluid pump, until the middle-deep well cross-linked polymer in drilling rod is coagulated
Glue sealing agent all replaces with drilling fluid, is then shut off drilling fluid pump and carries out standing building the pressure leak stopping 60 minutes；
(10) reopen drilling fluid pump and carry out pressure testing, if not occurring bottom pressure rising after pressure testing, close drilling fluid pump
Repeat step is (1) to (9) afterwards；
If (11) occurring bottom pressure rising after pressure testing, close drilling fluid pump continuation standing and build the pressure 20 minutes, then again
Start drilling fluid pump, and control the discharge capacity of drilling fluid pump for 0.3m3/min, by the middle-deep well cross-linked polymeric between well and drilling rod
Thing GEL USED FOR PLUGGING WELL LOST CIRCULATION all replaces with drilling fluid, and drilling fluid pump is closed after drilling fluid is returned out from well head and proceeds standing and builds the pressure
12 hours；Standing build the pressure 12 hours during every 30 minutes, to underground supplement a drilling fluid, returned again from well head to drilling fluid
Go out to stop；
(12) open drilling fluid pump and carry out leak stopping pressure-bearing test, the normal value returned to when the pump pressure of drilling fluid pump before leakage
When, proceed operation of drilling.
First, initial set, final setting time experiment are carried out to the sealing agent of the embodiment of the present invention two
The pre-hardening and final setting time of sealing agent at different temperatures is tested with reference to GB/T50080-2002 standard,
Record initial set and the final setting time such as table 1 of sealing agent.
Table 1
。
As can be seen from Table 1, at 30 DEG C, the sealing agent presetting period can reach 135 minutes, and final setting time can reach 420
Minute, but with the raising of temperature, gelling time quickly shortens.The presetting period is 21 minutes when wherein reaching 60 DEG C, reaches 120
DEG C when the presetting period be only 3min, substantially belonging to moment has started glue, but higher than 60 DEG C after final setting time become steady.
2nd, slit formation plugging test is carried out to the sealing agent of the embodiment of the present invention one to embodiment three
SY/T 5840-2007 are pressed in experiment《People's Republic of China's oil and gas industry standard well liquid is stifled with bridge joint
Leak material Experimental Method in Laboratory》Perform.The DLM-01 type sealing Analog Devices produced with Bohai Sea drilling project institute, can be heated up to 150
DEG C, 7.0MPa can be forced into.The vertical slit die plate of selection, thickness 5mm stitches high 50mm, slit width is 3mm.
The sealing agent heating-up temperature of embodiment one is 80 DEG C, and the sealing agent heating-up temperature of embodiment two is 120 DEG C, embodiment
Three sealing agent heating-up temperature is 140 DEG C, and the sealing agent 2000mL of the present invention is injected into test chamber, and sealing agent is quickly entered
Template gap is simultaneously flowed out from the lower part outlet of device, and record sealing agent stops the delivery time, as blocking time, and result of the test is converged
Total such as table 2 below.
Table 2
。
After blocking successfully above, 4 hours are stood respectively, clear water is then poured into, then embodiment one is still heated up to 80 DEG C
And constant temperature is kept, embodiment two still heats up to 120 DEG C and keeps constant temperature, and embodiment three still heats up to 140 DEG C and keeps permanent
Temperature, is forced under different pressures and carries out plugging test, is maintained 300 seconds under each pressure, observes leakage situation, judges closure effect
Really, result of the test is as shown in table 3.
Table 3
。
3rd, osmosis type plugging test is carried out to the sealing agent of the embodiment of the present invention one to embodiment three
SY/T 5840-2007 are pressed in experiment《People's Republic of China's oil and gas industry standard well liquid is stifled with bridge joint
Leak material Experimental Method in Laboratory》Perform.The DLM-01 type sealing Analog Devices produced with Bohai Sea drilling project institute, the filtering surface of casting bed
Product 2289mm2, casting bed thickness 35mm.
The sealing agent heating-up temperature of embodiment one is 80 DEG C, and the sealing agent heating-up temperature of embodiment two is 120 DEG C, embodiment
Three sealing agent heating-up temperature is 140 DEG C, and the sealing agent 2000mL of the present invention is injected into test chamber, and sealing agent is quickly entered
Casting bed simultaneously flows out from the lower part outlet of device, and record sealing agent stops the delivery time, as blocking time, result of the test collect as
Shown in table 4 below.
Table 4
。
Embodiment three does not have sealing agent outflow at 140 DEG C, and it is to block successfully that sealing agent, which penetrates into casting bed 3/4,.
After blocking successfully above, 4 hours are stood respectively, clear water is then poured into, then embodiment one is still heated up to 80 DEG C
And constant temperature is kept, embodiment two still heats up to 120 DEG C and keeps constant temperature, and embodiment three still heats up to 140 DEG C and keeps permanent
Temperature, is forced under different pressures and carries out plugging test, is maintained 300 seconds under each pressure, observes leakage situation, judges closure effect
Really, result of the test is as shown in table 5.
Table 5
。
4th, ultimate compressive ability test is carried out to the blob of viscose of the sealing agent formation of the embodiment of the present invention two
The sealing agent of the embodiment of the present invention two is taken to be gelled respectively at 140 DEG C 4 hours and 12 hours, to obtained blob of viscose point
Do not carry out mechanical pressurization, test causes its structure to be badly deformed loose pressure value.Result of the test is as shown in table 6.
Table 6
。
As can be seen that with the increase of gelling time, the blob of viscose compression strength of formation increases, and highest can be with resistance to compression 15MPa.
Purified cotton used of the invention is uniform loose, without impurity such as wood chip, bamboo scraps, silt, greasy dirt, metal objects white wadding
Shape thing.Its raw material is cotton linter, and main chemical compositions are cellulose, lignin and hemicellulose.It is by carbon, hydrogen, three kinds of oxygen
Element is constituted, its mass ratio constituted：Carbon 44.4%, hydrogen 6.17%, oxygen 49.39%.The formula of purified cotton is：（C6H1005）
N, n represent the degree of polymerization of cellulose, and the degree of polymerization is generally 12000~14000.
Composite Portland cement slurry composite Portland cement used of the present invention is given birth to for Beijing Jinyu cement Trade Co., Ltd.
The composite Portland cement of production（P.C）.
Hydrophilic finishing agent used of the invention is that the TD-5512 types that Shenzhen Tianding Fine Chemical Engineering Manufacturing Co., Ltd produces are durable
Property hydrophilic finishing agent.
It the foregoing is only the preferable possible embodiments of the present invention, non-therefore the limitation present invention patent protection model
Enclose.In addition to the implementation, the present invention can also have other embodiment.All use equivalent substitutions or the skill of equivalent transformation formation
Art scheme, all falls within the protection domain of application claims.The technical characteristic that the present invention is not described to the greatest extent can be by or using now
There is technology realization, will not be repeated here.
Claims (8)
1. a kind of method that use cross-linked polymer gel sealing agent carries out middle-deep well leak stopping, it is characterised in that successively including such as
Lower step：
(1) raw material, purified cotton sodium salt solution are prepared by following components and weight content：120 parts, acrylamide：（75~85）Part,
Ammonium persulfate：（13~17）Part, cerous sulfate：（2~5）Part, beta-D-mannuronic acid：4 parts, ammonium dihydrogen phosphate：（1~1.5）Part,
Composite Portland cement is starched：100 parts and mix type microfibre：（150~200）Part；The water ash of the composite Portland cement slurry
Than for 0.44；
(2) acrylamide is added into purified cotton sodium salt solution, carrying out high-speed stirred with 400r/min rotating speed makes both in 10 minutes
It is sufficiently mixed, moderate-speed mixer is then carried out with 300r/min rotating speed, 60 DEG C are heated to while moderate-speed mixer and constant temperature is kept；
(3) nitrogen is continually fed into step reaction product (2) and reaction vessel, is passed through nitrogen and is keeping middling speed to stir after 3 minutes
Mix and be maintained at 60 DEG C of constant temperature, be slowly added to ammonium persulfate particle, reaction until after particulate matter disappearance, continuing back flow reaction
1.5 hour；
(4) temperature is increased to 80 DEG C and keeps constant temperature, in the case where keeping moderate-speed mixer, be slowly added to cerous sulfate particle, be then shut off
The charge door of reaction vessel, lifts the charge of nitrogen, and it is 1.3MPa, back flow reaction 3 hours to keep the pressure in reaction vessel
Above until white emulsion shape is presented in reactant, cross-linked polymer gel is obtained；Detect the molecule of the cross-linked polymer gel
Amount is more than 4,000,000；
(5) in the state of moderate-speed mixer is kept, beta-D-mannuronic acid is slowly added into above-mentioned cross-linked polymer gel, plus
Enter to continue after finishing moderate-speed mixer 10 minutes, and it is 7~7.5 to adjust pH value；
(6) composite Portland cement slurry is added into step reaction product (5) and mixes type microfibre, moderate-speed mixer 15 minutes with
Above until well mixed；
(7) ammonium dihydrogen phosphate is added into step reaction product (6), moderate-speed mixer 10 minutes obtains middle-deep well cross-linked polymer
GEL USED FOR PLUGGING WELL LOST CIRCULATION；
(8) continue moderate-speed mixer after 10 minutes, start drilling fluid pump by above-mentioned middle-deep well cross-linked polymer gel sealing agent through drilling rod
It is delivered to drop ply, the discharge capacity of drilling fluid pump is 1.5m3/min, and 60~90m3 of continuous conveying；
(9) continue to convey drilling fluid into drilling rod using drilling fluid pump, until the middle-deep well cross-linked polymer gel in drilling rod is blocked up
Leakage agent all replaces with drilling fluid, is then shut off drilling fluid pump and carries out standing building the pressure leak stopping 60 minutes；
(10) reopen drilling fluid pump and carry out pressure testing, if not occurring bottom pressure rising after pressure testing, close weight after drilling fluid pump
Multiple step is (1) to (9)；
If (11) occurring bottom pressure rising after pressure testing, close drilling fluid pump continuation standing and build the pressure 20 minutes, be then again started up
Drilling fluid pump, and the discharge capacity of drilling fluid pump is controlled for 0.2~0.3m3/min, the middle-deep well between well and drilling rod is crosslinked poly-
Compound GEL USED FOR PLUGGING WELL LOST CIRCULATION all replaces with drilling fluid, and drilling fluid pump is closed after drilling fluid is returned out from well head and proceeds standing and suppresses
Pressure 12 hours；Standing build the pressure 12 hours during every 30 minutes, to underground supplement a drilling fluid, to drilling fluid again from well head
Return out stopping；
(12) open drilling fluid pump and carry out leak stopping pressure-bearing test, when the pump pressure of drilling fluid pump returns to the normal value before leakage, after
It is continuous to carry out operation of drilling.
2. use cross-linked polymer gel sealing agent according to claim 1 carries out the method for middle-deep well leak stopping, its feature
Be, step (1) in raw material components and weight content it is as follows, purified cotton sodium salt solution：120 parts, acrylamide：75 parts, over cure
Sour ammonium：13 parts, cerous sulfate：2 parts, beta-D-mannuronic acid：4 parts, ammonium dihydrogen phosphate：1 part, composite Portland cement slurry：100 parts
With mix type microfibre：150 parts.
3. use cross-linked polymer gel sealing agent according to claim 1 carries out the method for middle-deep well leak stopping, its feature
Be, step (1) in raw material components and weight content it is as follows, purified cotton sodium salt solution：120 parts, acrylamide：80 parts, mistake
Ammonium sulfate：15 parts, cerous sulfate：3 parts, beta-D-mannuronic acid：4 parts, ammonium dihydrogen phosphate：1.2 parts, composite Portland cement slurry：
100 parts and mix type microfibre：180 parts.
4. use cross-linked polymer gel sealing agent according to claim 1 carries out the method for middle-deep well leak stopping, its feature
Be, step (1) in raw material components and weight content it is as follows, purified cotton sodium salt solution：120 parts, acrylamide：85 parts, over cure
Sour ammonium：17 parts, cerous sulfate：5 parts, beta-D-mannuronic acid：4 parts, ammonium dihydrogen phosphate：1.5 parts, composite Portland cement slurry：100
Part and mix type microfibre：200 parts.
5. use cross-linked polymer gel sealing agent according to claim 1 carries out the method for middle-deep well leak stopping, its feature
It is, the preparation method of the purified cotton sodium salt is as follows：1. prepare the cotton fiber degree of polymerization for 12000~14000 purified cotton and
Concentration expressed in percentage by weight is 17.5~18% sodium hydroxide solution, and the weight ratio of purified cotton and sodium hydroxide solution is 5:2；2. will
In purified cotton input sodium hydroxide solution, stir and react more than 1.5 hours at 60 DEG C, until uniform white suspension is presented
Emulsion, obtains purified cotton sodium salt just solution；3. ultrasonic micro-vibration is carried out to solution at the beginning of purified cotton sodium salt 30 minutes, obtains purified cotton
Sodium salt solution, supersonic frequency is 20kHz~30kHz, and ultrasonication intensity is 2.0 W/cm2~3.0W/cm2.
6. use cross-linked polymer gel sealing agent according to claim 1 carries out the method for middle-deep well leak stopping, its feature
Be, it is described mix type microfibre by calcium carbonate crystal whisker and organic microfiber carry out it is uniform mix form, calcium carbonate crystal whisker and have
The mixing ratio of machine microfibre is 0.8:1.
7. use cross-linked polymer gel sealing agent according to claim 6 carries out the method for middle-deep well leak stopping, its feature
Be, 20~30 μm of the length of the calcium carbonate crystal whisker, 0.5~1 μm of diameter, pH value 9.0~9.5, modulus of elasticity be 410~
710GPa and tensile strength is not less than 2.058GPa；The organic microfiber is made up of polyester fiber and polypropylene fibre, polyester
The weight ratio of fiber and polypropylene fibre is 7:3；20~25 μm of the diameter of the polyester fiber, 6~9mm of length, extension at break
Rate >=15%, tensile strength >=960MPa and modulus of elasticity >=9000MPa；The length of the polypropylene fibre is 10~20mm,
Filament number≤2.2dtex, tensile strength >=660MPa, modulus of elasticity >=350MPa.
8. use cross-linked polymer gel sealing agent according to claim 7 carries out the method for middle-deep well leak stopping, its feature
It is, the polyester fiber and polypropylene fibre soak 3 hours at 60 DEG C in hydrophilic finishing agent.
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| CN105909240A (en) * | 2016-04-14 | 2016-08-31 | 中国海洋石油总公司 | Bottom hole pressure testing, polymer displacement front edge position monitoring and reservoir assessment method |
| CN109054778B (en) * | 2018-09-05 | 2021-03-16 | 中石化石油工程技术服务有限公司 | Water-based film forming agent, preparation method thereof, water-based drilling fluid and application thereof |
| CN110439498B (en) * | 2019-08-08 | 2021-09-28 | 中国石油集团渤海钻探工程有限公司 | Medium-deep well plugging method adopting plugging agent capable of delaying water absorption expansion |
| CN111255411B (en) * | 2020-04-23 | 2021-11-30 | 中石化石油工程技术服务有限公司 | Method for plugging high-temperature well by adopting core-shell type high-temperature-resistant plugging agent |
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