CN105112031B - A kind of method that use high molecular polymerization frozen glue sealing agent carries out shallow well leak stopping - Google Patents
A kind of method that use high molecular polymerization frozen glue sealing agent carries out shallow well leak stopping Download PDFInfo
- Publication number
- CN105112031B CN105112031B CN201510577429.1A CN201510577429A CN105112031B CN 105112031 B CN105112031 B CN 105112031B CN 201510577429 A CN201510577429 A CN 201510577429A CN 105112031 B CN105112031 B CN 105112031B
- Authority
- CN
- China
- Prior art keywords
- parts
- drilling fluid
- high molecular
- sealing agent
- frozen glue
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- 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
- C09K8/42—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells
- C09K8/46—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells containing inorganic binders, e.g. Portland cement
- C09K8/467—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells containing inorganic binders, e.g. Portland cement containing additives for specific purposes
-
- 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
- C09K2208/00—Aspects relating to compositions of drilling or well treatment fluids
- C09K2208/08—Fiber-containing well treatment fluids
-
- 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
- C09K2208/00—Aspects relating to compositions of drilling or well treatment fluids
- C09K2208/18—Bridging agents, i.e. particles for temporarily filling the pores of a formation; Graded salts
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Curing Cements, Concrete, And Artificial Stone (AREA)
- Sealing Material Composition (AREA)
Abstract
The present invention relates to a kind of method that use high molecular polymerization frozen glue sealing agent carries out shallow well leak stopping, raw material weight ratio is 120 parts of purified cotton sodium salt solution, 75~85 parts of acrylamide, 13~17 parts of ammonium persulfate, 2~5 parts of cerous sulfate, β D mannuronic acids（M）：4 parts, 1~1.5 part of ammonium dihydrogen phosphate, composite Portland cement starch 100 parts, 80~90 parts of talcum powder and mix 20 parts of type microfibre；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 heatproof resistance to compression.
Description
Technical field
The present invention relates to a kind of method that use high molecular polymerization frozen glue sealing agent carries out shallow well leak stopping, belong to oil drilling
Technical field.
Background technology
Leakage is the technical barrier frequently encountered in drilling process, can cause a large amount of losses of drilling fluid, cause drilling well into
This rising, while bottom pressure can be caused to change, induces the hair of the complex accidents such as borehole well instability, well slough, well kick, blowout
It is raw, seriously govern the raising of bit speed.
It is general using conventional stifled due to lacking new leakage stopping technology at present when oil drilling drilling strata misses section
Leak agent leak stopping.Processing shallow well leakage in the country's generally uses bridge joint leak stopping, and bridge joint leak stopping has economy, easy to use, construction peace
Full advantage, can solve the partial loss that is caused by hole and crack and leakage is returned in mistake.The bridge joint loss circulation material that the country is used
It is roughly divided into three classes：Hard fruit shell class, fibrous material and lamellar material.In Process of Leaking Stoppage, any kind material is independent
Use, 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, can just receive should
Some effects, but deepening continuously with drilling, the temperature on leakage stratum are also constantly being raised, and are immersed in the hard in mud
Shell class material and plant fiber material such as walnut shell, hazelnut shell, cotton seed hulls and sawdust etc., high temperature, high pressure and strong in well
Under conditions of caustic corrosion, over time, these materials will slowly soften, corrode, or even some materials can be burnt, and cause
Bridge joint intensity is set drastically to decline, it is easy to cause leak stopping failure or secondary leakage, it is impossible to fundamentally solve the problem of leak stopping.
Well depth is that 2000~3000m is referred to as shallow well, and downhole temperature is generally at 80 DEG C~100 DEG C.Although conventional blocking method
Effect has been played for the stoppage engineering of oil drilling, but there is shortcoming or deficiency simultaneously, temperature resistant capability is low, the term of validity is short, stifled
Leak inefficient, loss circulation material consumption big, plugging time length, leak stopping safety coefficient poor, down hole problem easily occur, these are scarce
Point directly affects probing development process, therefore traditional loss circulation material far from disclosure satisfy that growing Holes of Complicated Wells
Leak stopping demand, therefore it is very necessary to study a kind of shallow well sealing agent.
The content of the invention
It is an object of the present invention to overcome problems of the prior art to use high molecular polymerization frozen glue there is provided one kind
The method that sealing agent carries out shallow well leak stopping, leak stopping is reliable, and heat resisting and pressure resisting.
To solve above technical problem, a kind of use high molecular polymerization frozen glue sealing agent of the invention carries out shallow well leak stopping
Method, in turn includes the following steps：(1) raw material, purified cotton sodium salt solution are prepared by following components and weight content：120 parts, third
Acrylamide：（75~85）Part, ammonium persulfate：（13~17）Part, cerous sulfate：（2~5）Part, beta-D-mannuronic acid：4 parts, phosphoric acid
Ammonium dihydrogen：（1~1.5）Part, composite Portland cement slurry：100 parts, talcum powder：（80~90）Part and mix type microfibre：20
Part；The ratio of mud of the composite Portland cement slurry is 0.44；(2) acrylamide is added into purified cotton sodium salt solution, with
400r/min rotating speed, which carries out high-speed stirred, is sufficiently mixed both in 10 minutes, and then carrying out middling speed with 300r/min rotating speed stirs
Mix, 60 DEG C are heated to while moderate-speed mixer and constant temperature is kept；(3) persistently lead into step reaction product (2) and reaction vessel
Enter nitrogen, be passed through nitrogen and keeping moderate-speed mixer after 3 minutes and be maintained at 60 DEG C of constant temperature, be slowly added to ammonium persulfate particle,
Reaction is until after particulate matter disappearance, continue back flow reaction 1.5 hours；(4) temperature is increased to 80 DEG C and keeps constant temperature, kept
Under moderate-speed mixer, cerous sulfate particle is slowly added to, the charge door of reaction vessel is then shut off, the charge of nitrogen is lifted, kept
Pressure in reaction vessel is 1.3MPa, back flow reaction more than 3 hours until reactant presentation white emulsion shape, obtains macromolecule
It polymerize frozen glue；Detect the molecular weight of the high molecular polymerization frozen glue 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 high molecular polymerization frozen glue, addition continues moderate-speed mixer 10 minutes after finishing, and
It is 7~7.5 to adjust pH value；(6) composite Portland cement slurry, talcum powder are added into step reaction product (5) and to mix type micro-
Fiber, moderate-speed mixer more than 15 minutes are until well mixed；(7) ammonium dihydrogen phosphate, middling speed are added into step reaction product (6)
Stirring 10 minutes, obtains shallow well high molecular polymerization frozen glue sealing agent；(8) moderate-speed mixer is continued after 10 minutes, and starting drilling fluid pump will
Above-mentioned shallow well high molecular polymerization frozen glue sealing agent is through Drill-pipe conveyed to drop ply, and the discharge capacity of drilling fluid pump is 1.5m3/min, and continuously
Convey 60~90m3；(9) continue to convey drilling fluid into drilling rod using drilling fluid pump, until by the shallow well polyphosphazene polymer in drilling rod
Close frozen glue sealing agent and all replace with drilling fluid, be then shut off drilling fluid pump and carry out standing building the pressure leak stopping 60 minutes；(10) open again
Open drilling fluid pump and carry out pressure testing, if not occurring bottom pressure rising after pressure testing, repeat step is (1) to (9) after closing drilling fluid pump；
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 well
Liquid pump, and control the discharge capacity of drilling fluid pump for 0.2~0.3m3/min, the shallow well high molecular polymerization between well and drilling rod is frozen
Glue sealing agent all replaces with drilling fluid, closed after drilling fluid is returned out from well head drilling fluid pump proceed standing build the pressure it is 12 small
When；Standing build the pressure 12 hours during every 30 minutes, to underground supplement a drilling fluid, return out and stop from well head again to drilling fluid
Only；(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, continue
Progress is drilled operation.
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 high molecular polymerization frozen glue 4,000,000 crosslinkings described above, copolymerization, graft reaction very fully, be shape
Intensity into " block wall " provides guarantee.3. added in high molecular polymerization frozen glue after beta-D-mannuronic acid, β-D-MANNOSE aldehyde
The sodium ion of acid is exchanged with the amide groups in high molecular polymerization frozen glue, ionic compartmentation is carried out at carboxyl position, so as to be gelled
Reaction, forms blob of viscose.Beta-D-mannuronic acid viscosity when pH is reduced can increase, and there is viscosity thixotropic when pH is 6.7, have
Certain alkali resistance, when pH is 7~7.5, the blob of viscose of formation has more preferable shear thinning behavior, and advantage is provided for pumping.
4. composite Portland cement slurry can provide the intensity and anti-pressure ability of blob of viscose；After the gelling of high molecular polymerization frozen glue, if wherein
There is no enough bridge particles, the blob of viscose intensity of formation is only capable of reaching 1~2MPa, it is impossible to meet the pressurization sealing requirement of shallow well；
Talcum powder and mix type microfibre and can play a part of bridge particle, phase has been cross-linked to form with natural fiber using synthetic fibers
The net high-polymer polymer mutually wound, in underground, high molecular polymerization frozen glue slowly starts after gelling, complete gelation, forms blob of viscose
Intensity can reach 5MPa, can more than 100 DEG C of heatproof, the leak stopping needs of 2000~3000m of well depth shallow well can be met.This
Mix the adding proportion of type microfibre in invention so that sealing agent has highest intensity, if continuing raising mixes type microfibre
Weight ratio, the chemical crosslinking of gel chemistries material can be disturbed to act on the contrary, the bearing capacity of its leak stopping can be reduced on the contrary.5. plus
Enter the ammonium dihydrogen phosphate of ratio of the present invention, can both ensure by gelling control in suitable time range before gelling, leak stopping
Agent can be pumped to drop ply, can complete drilling rod before gelling again with being starched in well, additionally it is possible to sealing agent is reached leakage
It is gelled in time after layer so that leak stopping slurries stop to live in drop ply.Discharge capacity is used for 1.5m3/min when 6. pumping sealing agent,
Both avoided discharge capacity is excessive from causing the formation fracture for having occurred and that leakage further to expand under huge discharge, and can have been incited somebody to action again before initial set
Sealing agent is all made a gift to someone drop ply；For the situation of most of small leakages and middle leakage, the glue time is played with reference to gelling leak stopping, 60 are conveyed every time
~90m3 is the most appropriate.7. after sealing agent conveying drop ply, first complete to replace slurry in drilling rod using drilling fluid, suppressed subsequently into standing
Pressure, prevents high molecular polymerization frozen glue to be gelled in drilling rod, blocks the central duct of drilling rod.8. pressure testing does not show on bottom pressure
Rise, illustrate leak stopping failure, it is necessary to carry out leak stopping again；Occur bottom pressure rising after pressure testing, illustrate leak stopping success, it is necessary to stand
Build the pressure 20 minutes, 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 is in 0.2~0.3m3/min, and preventing discharge capacity excessive, the blob of viscose formation newly formed to drop ply is impacted and broken
It is broken, have adverse effect on, cause leak stopping to fail.9. after the completion of well is for slurry, continues standing and build the pressure 12 hours, wait blob of viscose to reach
To predetermined intensity, pressure-bearing experiment is then carried out, when the pump pressure of drilling fluid pump returns to the normal value before leakage, illustrates that leak stopping is complete
Full success, 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：4 parts, ammonium dihydrogen phosphate：1
Part, composite Portland cement slurry：100 parts, talcum powder：80 parts and mix type microfibre：20 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：4 parts, ammonium dihydrogen phosphate：
1.2 parts, composite Portland cement slurry：100 parts, talcum powder：85 parts and mix type microfibre：20 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：4 parts, ammonium dihydrogen phosphate：
1.5 parts, composite Portland cement slurry：100 parts, talcum powder：90 parts and mix type microfibre：20 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 high molecular polymerization frozen glue, mutually wind netted is cross-linked to form with the high molecular polymer in high molecular polymerization frozen glue
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 ratio 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；It is described poly-
The length of tacryl is 10~20mm, filament number≤2.2dtex, tensile strength >=660MPa, modulus of elasticity >=350MPa.
Polypropylene fibre can improve the intensity of " block wall ", improve the rebound performance of " block wall " after compressive deformation.Polyester fiber can
Improve anti-fatigue performance, cracking resistance and the high temperature stability performance of " block wall ", the tension of " block wall " can be effectively improved, resisted
Pressure, anti-shearing and impact strength, make 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 high molecular polymerization frozen glue
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 high molecular polymerization frozen glue sealing agent of the present invention carries out shallow well leak stopping, successively including following step
Suddenly：
(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：4 parts, ammonium dihydrogen phosphate：1 part, composite Portland cement slurry：100
Part, talcum powder：80 parts and mix type microfibre：20 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 high molecular polymerization frozen glue；Detect the molecule of the high molecular polymerization frozen glue
Amount is more than 4,000,000；
(5) in the state of moderate-speed mixer is kept, β-D-MANNOSE aldehyde is slowly added into above-mentioned high molecular polymerization frozen glue
Acid, addition continues moderate-speed mixer 10 minutes after finishing, and it is 7 to adjust pH value；
(6) composite Portland cement slurry, talcum powder are added into step reaction product (5) and mixes type microfibre, middling speed
Stirring more than 15 minutes is until well mixed；
(7) ammonium dihydrogen phosphate is added into step reaction product (6), moderate-speed mixer 10 minutes obtains shallow well polyphosphazene polymer
Close frozen glue sealing agent；
(8) continue moderate-speed mixer after 10 minutes, start drilling fluid pump by above-mentioned shallow well high molecular polymerization frozen glue sealing agent through boring
Bar is delivered 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 by the shallow well high molecular polymerization frozen glue in drilling rod
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 shallow well high molecular polymerization between well and drilling rod
Frozen glue sealing agent all replaces with drilling fluid, drilling fluid pump is closed after drilling fluid is returned out from well head proceeds standing and build the pressure 12
Hour；Standing build the pressure 12 hours during every 30 minutes, to underground supplement a drilling fluid, returned out again from well head to drilling fluid
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 high molecular polymerization frozen glue sealing agent of the present invention carries out shallow well leak stopping, successively including following step
Suddenly：
(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：4 parts, ammonium dihydrogen phosphate：1.2 parts, composite Portland cement slurry：100
Part, talcum powder：85 parts and mix type microfibre：20 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 high molecular polymerization frozen glue；Detect point of the high molecular polymerization frozen glue
Son amount is more than 4,000,000；
(5) in the state of moderate-speed mixer is kept, β-D-MANNOSE aldehyde is slowly added into above-mentioned high molecular polymerization frozen glue
Acid, addition continues moderate-speed mixer 10 minutes after finishing, and it is 7.5 to adjust pH value；
(6) composite Portland cement slurry, talcum powder are added into step reaction product (5) and mixes type microfibre, middling speed
Stirring more than 15 minutes is until well mixed；
(7) ammonium dihydrogen phosphate is added into step reaction product (6), moderate-speed mixer 10 minutes obtains shallow well polyphosphazene polymer
Close frozen glue sealing agent；
(8) continue moderate-speed mixer after 10 minutes, start drilling fluid pump by above-mentioned shallow well high molecular polymerization frozen glue sealing agent through boring
Bar is delivered 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 by the shallow well high molecular polymerization frozen glue in drilling rod
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, by the shallow well polyphosphazene polymer between well and drilling rod
Close frozen glue sealing agent and all replace with drilling fluid, 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 three
The method that a kind of use high molecular polymerization frozen glue sealing agent of the present invention carries out shallow well leak stopping, successively including following step
Suddenly：
(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：4 parts, ammonium dihydrogen phosphate：1.5 parts, composite Portland cement slurry：100
Part, talcum powder：90 parts and mix type microfibre：20 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 high molecular polymerization frozen glue；Detect point of the high molecular polymerization frozen glue
Son amount is more than 4,000,000；
(5) in the state of moderate-speed mixer is kept, β-D-MANNOSE aldehyde is slowly added into above-mentioned high molecular polymerization frozen glue
Acid, addition continues moderate-speed mixer 10 minutes after finishing, and adjusts pH value 7.5；
(6) composite Portland cement slurry, talcum powder are added into step reaction product (5) and mixes type microfibre, middling speed
Stirring more than 15 minutes is until well mixed；
(7) ammonium dihydrogen phosphate is added into step reaction product (6), moderate-speed mixer 10 minutes obtains shallow well polyphosphazene polymer
Close frozen glue sealing agent；
(8) continue moderate-speed mixer after 10 minutes, start drilling fluid pump by above-mentioned shallow well high molecular polymerization frozen glue sealing agent through boring
Bar is delivered 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 by the shallow well high molecular polymerization frozen glue in drilling rod
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 shallow well high molecular polymerization between well and drilling rod
Frozen glue sealing agent all replaces with drilling fluid, drilling fluid pump is closed after drilling fluid is returned out from well head proceeds standing and build the pressure 12
Hour；Standing build the pressure 12 hours during every 30 minutes, to underground supplement a drilling fluid, returned out again from well head to drilling fluid
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 130 minutes, and final setting time can reach 410
Minute, but with the raising of temperature, gelling time quickly shortens.The presetting period is 20 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 100 DEG C, embodiment
Three sealing agent heating-up temperature is 120 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 100 DEG C and keeps constant temperature, and embodiment three still heats up to 120 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 100 DEG C, embodiment
Three sealing agent heating-up temperature is 120 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
。
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 100 DEG C and keeps constant temperature, and embodiment three still heats up to 120 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
。
As can be seen that the sealing agent of the present invention is at 100 DEG C, bearing capacity can reach 5MPa, can meet shallow well leak stopping
Need.
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 high molecular polymerization frozen glue sealing agent carries out shallow well leak stopping, it is characterised in that successively including as follows
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, talcum powder：（80~90）Part and mix type microfibre：20 parts；The complex silicate salt solution
The ratio of mud of mud is 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, high molecular polymerization frozen glue is obtained；Detect the molecule of the high molecular polymerization frozen glue
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 high molecular polymerization frozen glue, 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, talcum powder are added into step reaction product (5) and mixes type microfibre, moderate-speed mixer
More than 15 minutes until well mixed；
(7) ammonium dihydrogen phosphate is added into step reaction product (6), and moderate-speed mixer 10 minutes obtains shallow well high molecular polymerization jelly
Glue sealing agent；
(8) continue moderate-speed mixer after 10 minutes, start drilling fluid pump above-mentioned shallow well high molecular polymerization frozen glue sealing agent is defeated through drilling rod
Deliver 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 by the shallow well high molecular polymerization frozen glue leak stopping in drilling rod
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, by the shallow well polyphosphazene polymer between well and drilling rod
Close frozen glue sealing agent and all replace with drilling fluid, 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, 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. the method that use high molecular polymerization frozen glue sealing agent according to claim 1 carries out shallow well leak stopping, its feature exists
In, step (1) in raw material components and weight content it is as follows, purified cotton sodium salt solution：120 parts, acrylamide：75 parts, persulfuric acid
Ammonium：13 parts, cerous sulfate：2 parts, beta-D-mannuronic acid：4 parts, ammonium dihydrogen phosphate：1 part, composite Portland cement slurry：100 parts,
Talcum powder：80 parts and mix type microfibre：20 parts.
3. the method that use high molecular polymerization frozen glue sealing agent according to claim 1 carries out shallow well leak stopping, its feature exists
In, step (1) in raw material components and weight content it is as follows, purified cotton sodium salt solution：120 parts, acrylamide：80 parts, over cure
Sour ammonium：15 parts, cerous sulfate：3 parts, beta-D-mannuronic acid：4 parts, ammonium dihydrogen phosphate：1.2 parts, composite Portland cement slurry：100
Part, talcum powder：85 parts and mix type microfibre：20 parts.
4. the method that use high molecular polymerization frozen glue sealing agent according to claim 1 carries out shallow well leak stopping, its feature exists
In, step (1) in raw material components and weight content it is as follows, purified cotton sodium salt solution：120 parts, acrylamide：85 parts, persulfuric acid
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, talcum powder：90 parts and mix type microfibre：20 parts.
5. the method that use high molecular polymerization frozen glue sealing agent according to claim 1 carries out shallow well leak stopping, its feature exists
In the preparation method of the purified cotton sodium salt is as follows：1. it is 12000~14000 purified cotton and again to prepare the cotton fiber degree of polymerization
The weight ratio of the sodium hydroxide solution that amount percentage concentration is 17.5~18%, purified cotton and sodium hydroxide solution is 5:2；2. by essence
In cotton input sodium hydroxide solution processed, stir and react more than 1.5 hours at 60 DEG C, until uniform white suspension breast is presented
Liquid, 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
Salting liquid, supersonic frequency is 20kHz~30kHz, and ultrasonication intensity is 2.0 W/cm2~3.0W/cm2.
6. the method that use high molecular polymerization frozen glue sealing agent according to claim 1 carries out shallow well leak stopping, its feature exists
In, 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 organic
The mixing ratio of microfibre is 0.8:1.
7. the method that use high molecular polymerization frozen glue sealing agent according to claim 6 carries out shallow well leak stopping, its feature exists
In, 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 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. the method that use high molecular polymerization frozen glue sealing agent according to claim 7 carries out shallow well leak stopping, its feature exists
In the polyester fiber and polypropylene fibre soak 3 hours at 60 DEG C in hydrophilic finishing agent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510577429.1A CN105112031B (en) | 2015-09-11 | 2015-09-11 | A kind of method that use high molecular polymerization frozen glue sealing agent carries out shallow well leak stopping |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510577429.1A CN105112031B (en) | 2015-09-11 | 2015-09-11 | A kind of method that use high molecular polymerization frozen glue sealing agent carries out shallow well leak stopping |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105112031A CN105112031A (en) | 2015-12-02 |
| CN105112031B true CN105112031B (en) | 2017-10-17 |
Family
ID=54660153
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510577429.1A Active CN105112031B (en) | 2015-09-11 | 2015-09-11 | A kind of method that use high molecular polymerization frozen glue sealing agent carries out shallow well leak stopping |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105112031B (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| US11981601B2 (en) | 2021-01-05 | 2024-05-14 | Saudi Arabian Oil Company | In-situ polyphosphazene generation in cement for improved elastic properties |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101250398A (en) * | 2008-03-25 | 2008-08-27 | 施晓红 | Well drilling leak-proof sealing agent |
| CN101857398A (en) * | 2009-04-08 | 2010-10-13 | 中国石油天然气股份有限公司 | Strong wall-building composite plugging agent |
| CN102382632A (en) * | 2010-09-03 | 2012-03-21 | 中国石油化工股份有限公司 | Pretreating agent preventing leaking stoppage from being diluted by formation water and preparation method and application thereof |
| CN104726078A (en) * | 2015-03-13 | 2015-06-24 | 商南天和泥浆有限公司 | Gel plugging agent and preparation method thereof |
-
2015
- 2015-09-11 CN CN201510577429.1A patent/CN105112031B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101250398A (en) * | 2008-03-25 | 2008-08-27 | 施晓红 | Well drilling leak-proof sealing agent |
| CN101857398A (en) * | 2009-04-08 | 2010-10-13 | 中国石油天然气股份有限公司 | Strong wall-building composite plugging agent |
| CN102382632A (en) * | 2010-09-03 | 2012-03-21 | 中国石油化工股份有限公司 | Pretreating agent preventing leaking stoppage from being diluted by formation water and preparation method and application thereof |
| CN104726078A (en) * | 2015-03-13 | 2015-06-24 | 商南天和泥浆有限公司 | Gel plugging agent and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 基于增温抗粘的魔芋粉-丙烯酰胺接枝共聚改性研究;董艳，等;《安徽农业科学》;20080520;第36卷(第15期);第6154-6156页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105112031A (en) | 2015-12-02 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105114032B (en) | A kind of method that use cross-linked polymer gel sealing agent carries out middle-deep well leak stopping | |
| CN102146280B (en) | Controllable expanded plugging agent | |
| CN104861953A (en) | Oil field fracture temporary plugging agent and preparation method thereof | |
| CN104178102A (en) | Cross-linkable high-temperature-resistant residue-free polybasic copolymerizable fracturing fluid and preparation method thereof | |
| CN109575893B (en) | Temporary plugging fluid for carbonate rock acid fracturing steering | |
| CN104388066B (en) | Preparation method of plugging agent for drilling fluid | |
| Su et al. | Thermoviscosifying smart polymers for oil and gas production: state of the art | |
| CN108865088B (en) | Temporary plugging agent, preparation method thereof, drilling fluid and application of drilling fluid in plugging of fractured reservoir while drilling | |
| CN110079288B (en) | Expansive temporary plugging agent and preparation method thereof | |
| CN104710973A (en) | Non-residue polymer fracturing fluid | |
| CN105219365B (en) | Middle-deep well cross-linked polymer gel sealing agent and preparation method thereof | |
| CN105112031B (en) | A kind of method that use high molecular polymerization frozen glue sealing agent carries out shallow well leak stopping | |
| CN109796950A (en) | A kind of adaptively pinpoint blocks composite turning agent and its application | |
| CN113512414B (en) | Delayed crosslinking type high-temperature-resistant low-friction-resistance aggravated guanidine gum fracturing fluid and application method thereof | |
| CN114479778A (en) | Plugging agent for oil-based drilling fluid and application | |
| CN105086966B (en) | Shallow well high molecular polymerization frozen glue sealing agent and preparation method thereof | |
| CN106958438A (en) | A kind of polymer flooding blocks the method for removing blockage of well | |
| CN106928948A (en) | A kind of uncrosslinked gel leak stopping system | |
| CN106479462A (en) | A kind of blocking agent and preparation method thereof and oil well casing leak stopping envelope alter method | |
| CN108587587B (en) | High-strength degradable temporary plugging ball for oil and gas well as preparation method and application of temporary plugging ball | |
| CN112980407A (en) | Temperature-controllable gel plugging agent and preparation method and application thereof | |
| CN105713594A (en) | Viscous acid and preparation method thereof | |
| CN110305644B (en) | Preparation and application of leakage-reducing flexible colloidal particle well-flushing fluid | |
| CN110396398B (en) | Temperature control type curing agent for ultra-high temperature oil-based drilling fluid and preparation method thereof | |
| CN116083063B (en) | Delayed expansion plugging system and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |