CN108130062A - A kind of water-soluble liquid rubber plug and preparation method thereof of quickly degrading certainly - Google Patents
A kind of water-soluble liquid rubber plug and preparation method thereof of quickly degrading certainly Download PDFInfo
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- CN108130062A CN108130062A CN201810057971.8A CN201810057971A CN108130062A CN 108130062 A CN108130062 A CN 108130062A CN 201810057971 A CN201810057971 A CN 201810057971A CN 108130062 A CN108130062 A CN 108130062A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/42—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells
- C09K8/44—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells containing organic binders only
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/42—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells
- C09K8/426—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells for plugging
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/50—Compositions for plastering borehole walls, i.e. compositions for temporary consolidation of borehole walls
- C09K8/504—Compositions based on water or polar solvents
- C09K8/506—Compositions based on water or polar solvents containing organic compounds
- C09K8/508—Compositions based on water or polar solvents containing organic compounds macromolecular compounds
- C09K8/512—Compositions based on water or polar solvents containing organic compounds macromolecular compounds containing cross-linking agents
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Abstract
The present invention discloses a kind of water-soluble liquid rubber plug and preparation method thereof of quickly degrading certainly, belongs to oil gas development technology field.The quick water-soluble liquid rubber plug of degradation certainly comprises the following raw materials by weight percent：Thickening agent 2.5 3.0%, crosslinking agent 7.5 8.0%, crosslinking accelerator 8.5 9%, solidification intensifier 1.5 2.0%, rubber plug degradation agent 2.0 2.5%, rubber plug degradation of promoter 0.1 0.2%, surplus is water, wherein, the thickening agent is konjaku glucomannan and the mixture of welan gum or diutan.Liquid gum plug provided by the invention, hardening time, viscosity was low before rubber plug curing, good fluidity, easily pump is noted within 1 2h；High strength after curing, bearing capacity are strong；Automatically degradable aquation in 5 12h after curing, viscosity is low after degradation, good fluidity, directly can go out pit shaft with clear water, post processing is simple.
Description
Technical field
The invention belongs to oil gas development technology fields, and in particular to a kind of quickly from degradation water-soluble liquid rubber plug and its system
Preparation Method.
Background technology
In oil-gas field development, in some oil/gas well development operations, for equilibrium strata pressure, it is necessary to using highdensity
Well killing fluid carry out kill-job, it is ensured that the oil gas in stratum does not enter pit shaft, avoid pit shaft, blowout generation.But highdensity pressure
Well liquid is easily accessible stratum, too big to formation damage or even can block oil-gas Layer, and well is killed, influences oil and gas production.
Secondly, when some oil/gas wells carry out pressing crack construction, need using the machine tools such as bridge plug, packer to pit shaft or
Person's oil jacket annular space part is blocked, but machine plugging has needed lower tubular column, and sand plug such as occur in complex procedures, is blocked
Tool can be difficult, and increase construction risk.
In order to solve the above problem in oil and gas development, liquid gum plug is studied exploitation and gradually makees in oil/gas well in recent years
It is used in industry.Liquid gum plug can replace high density well control fluids to carry out kill-job operation, can also mechanical bridge plug be replaced to carry out staged fracturing,
Or mechanical packer is replaced to carry out pressing crack construction.But also there are gel breaking is difficult, the short time to glue for existing liquid gum plug
Degree increases the problems such as fast, pump note is difficult, for example, 106905940 A of Chinese patent CN disclose a kind of middle-high density elastic liquid
Rubber plug and method for well fixing employ two kinds of systems of guanidine glue and acrylamide and mix crosslinked method, it is necessary to be destroyed by external impacts
Rubber plug particle could degrade, and then destroy uneven, easy shape with brine well killing fluid circulation flushing, complex process, and rubber plug again
Into bulk rubber plug, post-processing difficulty being increased, and the crosslinking of acrylamide system is too fast, viscosity increases soon rubber plug in a short time,
Cause pump note difficult；101270277 A of Chinese patent CN disclose a kind of self-breaking glue solution body rubber plug horizontal well in segments perforating and fracturing
Construction technology and rubber plug prepare base fluid, then be crosslinked with potassium bichromate using hydroxypropyl guar, tonka-bean angle, borax and ammonium persulfate
Rubber plug is prepared, frozen glue can be quickly formed at normal temperatures after hydroxypropyl guar gum, tonka-bean angle and borax mix in water, it is difficult to hand over again
Connection, and viscosity is very big, pump note is difficult；102061152 A of Chinese patent CN disclose a kind of high controllable rubber breaking breaking agent for chemical temporary-plugging of intensity
Liquid gum plug forms rubber plug using acrylamide system cross-linked polymeric, and construction terminates that glue can be broken automatically, and crosslinking time is short, pressure-bearing
Intensity is high, but acrylamide polymerization-filling object breaks glue difficulty, post processing trouble；103160261 A of Chinese patent CN disclose one
The preparation of kind downhole intelligent rubber plug and its application method, use acrylamide and acrylic acid to receive as raw material, add in initiator sulfurous
Sour sodium synthesizes rubber plug raw material, then prepares base fluid, stablizing with cross-linking agents forming properties and can break glue automatically in setting time
Rubber plug, but need to synthesize rubber plug raw material, complex process in advance.
Invention content
In view of the defects existing in the prior art, the present invention provides a kind of quickly from degradation water-soluble liquid rubber plug and its preparation
Method, the rubber plug hardening time is adjustable, can cure in 1-2h, can degrade automatically after curing.
A kind of water-soluble liquid rubber plug of quickly degrading certainly, comprises the following raw materials by weight percent（According to 100% meter）：
Thickening agent 2.5-3.0%, crosslinking agent 7.5-8.0%, crosslinking accelerator 8.5-9%, solidification intensifier 1.5-2.0%, rubber plug degradation agent
2.0-2.5%, rubber plug degradation of promoter 0.1-0.2%, surplus is water, wherein, the thickening agent is konjaku glucomannan and Brunei
The mixture of glue or diutan.
The konjaku glucomannan and the mass ratio of welan gum or diutan are（3-4）：（1-2）.
The rubber plug degradation of promoter is dithiothreitol (DTT).
The solidification intensifier for carboxycellulose grafted propylene hydrochlorate, in starch-grafted acrylonitrile saponification object extremely
Few one kind.
The carboxycellulose grafted propylene hydrochlorate is the spherical CCPACP that grain size is 1.0-1.5mmKSH- II water-absorbing resin.
The starch-grafted acrylonitrile saponification object is H-SPAN water-absorbing resins.
The crosslinking agent is the one or two kinds of of titanium tetrachloride, triethoxysilane and alchlor.
The crosslinking accelerator is at least one of light magnesium oxide or super fine zinc oxide, and the super fine zinc oxide is put down
Equal grain size is 1 micron.
The rubber plug degradation agent is at least one of sulfamic acid microcapsules or solid nitric acid microcapsules, the amino
Sulfonic acid microcapsules and solid nitric acid microcapsules are prepared using boiling granulating technology.
The above-mentioned quick preparation method from water-soluble liquid rubber plug of degrading, the method are：In rotating speed 4000-5000r/
Under the stirring condition of min, water, thickening agent, crosslinking accelerator, crosslinking agent, rubber plug degradation agent, rubber plug degradation promotion are sequentially added
Agent, solidification intensifier, are added while stirring, and it is spare that 3-5min is stirred for after addition.
It is low for viscosity before ensuring rubber plug plastic since the effect of each raw material is different, good fluidity, it is impossible to which feed change adds
Add sequence.
Advantages of the present invention：
1. liquid gum plug provided by the invention can mildly be constructed according to well need adjust hardening time, hardening time 1-2h with
Interior, the additive amount of adjustment thickening agent, crosslinking agent and crosslinking accelerator, dosage difference hardening time is different, viscosity before rubber plug curing
Low, good fluidity is easily pumped and is noted, and will not occur the accident that viscosity is excessive and construction fails during pump note；
2. the liquid gum plug automatically degradable aquation in 5-12h after hardening, degradation time can be by adjusting rubber plug degradation agent
It is adjusted with the additive amount of rubber plug degradation of promoter, without additionally adding in other rush degradation agents, simplifies construction process, simultaneously
Viscosity is low after degradation, good fluidity, directly can go out pit shaft with clear water, post processing is simple；
3. the liquid gum plug high strength after curing, bearing capacity is strong, and 30- can be born by injecting 1000kg liquid gum plugs in the wellbore
More than 33MPa pressure differences can meet oil/gas well kill-job and fracturing plugging needs；
4. using biodegradable carboxy methyl cellulose or starch conversion high hydroscopic resin, improve rubber plug intensity and
Biological degradability has environment friendly.
Specific embodiment
The sulfamic acid microcapsules and solid nitric acid microcapsules used in the present invention are prepared using boiling granulating technology
's.
Embodiment 1
A kind of water-soluble liquid rubber plug of quickly degrading certainly, comprises the following raw materials by weight percent（According to 100% meter）：Thickening
Agent 2.5%, crosslinking agent 7.5%, crosslinking accelerator 9%, solidification intensifier 1.5%, rubber plug degradation agent 2.5%, rubber plug degradation of promoter
0.1%, surplus is water,
Wherein, the thickening agent is mass ratio 3:1 konjaku glucomannan and the mixture of welan gum；
The rubber plug degradation of promoter is dithiothreitol (DTT)；
The solidification intensifier is the spherical CCPACP that grain size is 1.0-1.5mmKSH- II water-absorbing resin, CCPACPKSH- II water suction
Resin is a kind of carboxycellulose grafted propylene hydrochlorate；
The crosslinking agent is titanium tetrachloride, the mixture of triethoxysilane, wherein, titanium tetrachloride accounts for described quickly from degradation water
The 7.0% of insoluble liquid rubber plug gross mass, triethoxysilane account for described quick from water-soluble liquid rubber plug gross mass of degrading
0.5%；
The crosslinking accelerator is the super fine zinc oxide that average grain diameter is 1 micron；
The rubber plug degradation agent is sulfamic acid microcapsules；
The above-mentioned quick preparation method from water-soluble liquid rubber plug of degrading, the method are：Rotating speed 4000-5000r/min's
Under stirring condition, water, thickening agent, crosslinking accelerator, crosslinking agent, rubber plug degradation agent, rubber plug degradation of promoter, curing are sequentially added
Reinforcing agent adds while stirring, and it is spare that 3-5min is stirred for after addition.
The quick viscosity from before degradation water-soluble liquid rubber plug, plastic is 16mPas, good fluidity, when curing for 60 DEG C
Between for 1.5h, the pressure difference of 33MPa can be born after curing, is degraded automatically after 7h, viscosity 8mPas after degradation.
Embodiment 2
A kind of water-soluble liquid rubber plug of quickly degrading certainly, comprises the following raw materials by weight percent（According to 100% meter）：Thickening
Agent 3.0%, crosslinking agent 8.0%, crosslinking accelerator 8.5%, solidification intensifier 2.0%, rubber plug degradation agent 2.5%, rubber plug degradation of promoter
0.12%, surplus is water,
Wherein, it is 4 that the thickening agent, which is mass ratio,:1 konjaku glucomannan and the mixture of diutan；
The rubber plug degradation of promoter is dithiothreitol (DTT)；
The solidification intensifier is H-SPAN water-absorbing resins, and H-SPAN water-absorbing resins are starch-grafted acrylonitrile saponification object；
Mixture of the crosslinking agent for triethoxysilane and alchlor, wherein, triethoxysilane account for it is described it is quick from
The 0.8% of water-soluble liquid rubber plug gross mass of degrading, alchlor account for described quick from water-soluble liquid rubber plug gross mass of degrading
7.2%；
The crosslinking accelerator is light magnesium oxide；
The rubber plug degradation agent is solid nitric acid microcapsules；
The preparation method is the same as that of Example 1 for the above-mentioned quick rubber plug of degradation water-soluble liquid certainly.
The quick viscosity from before degradation water-soluble liquid rubber plug, plastic is 18mPas, good fluidity, when curing for 60 DEG C
Between for 1.5h, the pressure difference of 32MPa can be born after curing, is degraded automatically after 6.5h, viscosity 9mPas after degradation.
Embodiment 3
A kind of water-soluble liquid rubber plug of quickly degrading certainly, comprises the following raw materials by weight percent：Thickening agent 2.8%, crosslinking agent
8.0%, crosslinking accelerator 8.5%, solidification intensifier 2.0%, rubber plug degradation agent 2.5%, rubber plug degradation of promoter 0.15%, surplus is
Water,
Wherein, it is 3 that the thickening agent, which is mass ratio,:2 konjaku glucomannan and the mixture of welan gum；
The rubber plug degradation of promoter is dithiothreitol (DTT)；
The solidification intensifier is H-SPAN water-absorbing resins, and H-SPAN water-absorbing resins are starch-grafted acrylonitrile saponification objects；
Mixture of the crosslinking agent for triethoxysilane and alchlor, wherein, triethoxysilane account for it is described it is quick from
The 0.6% of water-soluble liquid rubber plug gross mass of degrading, alchlor account for described quick from water-soluble liquid rubber plug gross mass of degrading
7.4%；
The crosslinking accelerator is light magnesium oxide；
The rubber plug degradation agent is the mixture of sulfamic acid microcapsules and solid nitric acid microcapsules, wherein, the micro- glue of sulfamic acid
Capsule accounts for the 1.0% of the quick water-soluble liquid rubber plug gross mass of degradation certainly, and solid nitric acid microcapsules account for described quickly from degradation water
The 1.5% of insoluble liquid rubber plug gross mass.
The preparation method is the same as that of Example 1.
The quick viscosity from before degradation water-soluble liquid rubber plug, plastic is 18mPas, good fluidity, when curing for 70 DEG C
Between for 80min, the pressure difference of 31MPa can be born after curing, is degraded automatically after 6.0h, viscosity 11mPas after degradation.
Embodiment 4
A kind of water-soluble liquid rubber plug of quickly degrading certainly, comprises the following raw materials by weight percent：Thickening agent 3.0%, crosslinking agent
7.6%, crosslinking accelerator 8.5%, solidification intensifier 1.5%, rubber plug degradation agent 2.4%, rubber plug degradation of promoter 0.1%, surplus is
Water,
Wherein, it is 4 that the thickening agent, which is mass ratio,:2 konjaku glucomannan and the mixture of welan gum；
The rubber plug degradation of promoter is dithiothreitol (DTT)；
The solidification intensifier is the spherical CCPACP that grain size is 1.0-1.5mmKSH- II water-absorbing resin, CCPACPKSH- II water suction
Resin is a kind of carboxycellulose grafted propylene hydrochlorate；
The crosslinking agent is the mixture of titanium tetrachloride and triethoxysilane, wherein, titanium tetrachloride accounts for described quick from degradation
The 7.0% of water-soluble liquid rubber plug gross mass, triethoxysilane account for described quick from water-soluble liquid rubber plug gross mass of degrading
0.6%；
The crosslinking accelerator is the super fine zinc oxide that average grain diameter is 1 micron；
The rubber plug degradation agent is sulfamic acid microcapsules；
The preparation method is the same as that of Example 1.
The quick viscosity from before degradation water-soluble liquid rubber plug, plastic is 20mPas, good fluidity, when curing for 80 DEG C
Between for 1h, the pressure difference of 32MPa can be born after curing, is degraded automatically after 5.5h, viscosity 10mPas after degradation.
Embodiment 5
A kind of water-soluble liquid rubber plug of quickly degrading certainly, comprises the following raw materials by weight percent：Thickening agent 2.7%, crosslinking agent
7.8%, crosslinking accelerator 8.7%, solidification intensifier 1.8%, rubber plug degradation agent 2.3%, rubber plug degradation of promoter 0.2%, surplus is
Water,
Wherein, it is 3.5 that the thickening agent, which is mass ratio,:1 konjaku glucomannan and the mixture of diutan；
The rubber plug degradation of promoter is dithiothreitol (DTT)；
The solidification intensifier is the spherical CCPACP that grain size is 1.0-1.5mmKSH- II water-absorbing resin and H-SPAN water-absorbing resins
Mixture, wherein, CCPACPKSH- II water-absorbing resin is a kind of carboxycellulose grafted propylene hydrochlorate, H-SPAN water-absorbing resins
It is a kind of starch-grafted acrylonitrile saponification object；Wherein, CCPACPKSH- II water-absorbing resin accounts for described quick water-soluble from degrading
0.8%, the H-SPAN water-absorbing resins of liquid gum plug gross mass account for described quick from water-soluble liquid rubber plug gross mass of degrading
1.0%；
The crosslinking agent is titanium tetrachloride；
The mixture for the super fine zinc oxide that the crosslinking accelerator is light magnesium oxide and average grain diameter is 1 micron, wherein, lightweight
Magnesia accounts for the 1.7% of the quick water-soluble liquid rubber plug gross mass of degradation certainly, and super fine zinc oxide accounts for described quickly from degradation water
The 7.0% of insoluble liquid rubber plug gross mass；
The rubber plug degradation agent is sulfamic acid microcapsules；
The preparation method is the same as that of Example 1.
The quick viscosity from before degradation water-soluble liquid rubber plug, plastic is 18mPas, good fluidity, when curing for 70 DEG C
Between for 1h, the pressure difference of 33MPa can be born after curing, is degraded automatically after 5.5h, viscosity 9mPas after degradation.
Embodiment 6
A kind of water-soluble liquid rubber plug of quickly degrading certainly, comprises the following raw materials by weight percent：Thickening agent 2.5%, crosslinking agent
7.5%, crosslinking accelerator 8.7%, solidification intensifier 1.7%, rubber plug degradation agent 2.2%, rubber plug degradation of promoter 0.15%, surplus is
Water,
Wherein, it is 3 that the thickening agent, which is mass ratio,:2 konjaku glucomannan and the mixture of diutan；
The rubber plug degradation of promoter is dithiothreitol (DTT)；
The solidification intensifier is the spherical CCPACP that grain size is 1.0-1.5mmKSH- II water-absorbing resin, CCPACPKSH- II inhales
Water-resin is carboxycellulose grafted propylene hydrochlorate；
The crosslinking agent is triethoxysilane；
The crosslinking accelerator is light magnesium oxide；
The rubber plug degradation agent is solid nitric acid microcapsules；
The preparation method is the same as that of Example 1.
The quick viscosity from before degradation water-soluble liquid rubber plug, plastic is 18mPas, good fluidity, when curing for 70 DEG C
Between for 80min, the pressure difference of 32MPa can be born after curing, is degraded automatically after 6h, viscosity 9mPas after degradation.
Claims (10)
- It is 1. a kind of quickly from degradation water-soluble liquid rubber plug, it is characterised in that：It comprises the following raw materials by weight percent：Thickening Agent 2.5-3.0%, crosslinking agent 7.5-8.0%, crosslinking accelerator 8.5-9%, solidification intensifier 1.5-2.0%, rubber plug degradation agent 2.0- 2.5%, rubber plug degradation of promoter 0.1-0.2%, surplus is water,Wherein, the thickening agent is konjaku glucomannan and the mixture of welan gum or diutan.
- It is 2. according to claim 1 quick from degradation water-soluble liquid rubber plug, it is characterised in that：The konjaku glucomannan Mass ratio with welan gum or diutan is（3-4）：（1-2）.
- It is 3. according to claim 1 quick from degradation water-soluble liquid rubber plug, it is characterised in that：The rubber plug degradation promotes Agent is dithiothreitol (DTT).
- It is 4. according to claim 1 quick from degradation water-soluble liquid rubber plug, it is characterised in that：The solidification intensifier is At least one of carboxycellulose grafted propylene hydrochlorate, starch-grafted acrylonitrile saponification object.
- It is 5. according to claim 4 quick from degradation water-soluble liquid rubber plug, it is characterised in that：The carboxycellulose connects Branch acrylates is the spherical CCPACP that grain size is 1.0-1.5mmKSH- II water-absorbing resin.
- It is 6. according to claim 4 quick from degradation water-soluble liquid rubber plug, it is characterised in that：The starch-grafted propylene Nitrile saponification object is H-SPAN water-absorbing resins.
- It is 7. according to claim 1 quick from degradation water-soluble liquid rubber plug, it is characterised in that：The crosslinking agent is tetrachloro Change the one or two kinds of of titanium, triethoxysilane and alchlor.
- It is 8. according to claim 1 quick from degradation water-soluble liquid rubber plug, it is characterised in that：The crosslinking accelerator is At least one of light magnesium oxide or super fine zinc oxide, the average grain diameter of the super fine zinc oxide is 1 micron.
- It is 9. according to claim 1 quick from degradation water-soluble liquid rubber plug, it is characterised in that：The rubber plug degradation agent is At least one of sulfamic acid microcapsules or solid nitric acid microcapsules, the sulfamic acid microcapsules and the micro- glue of solid nitric acid Capsule is prepared using boiling granulating technology.
- 10. claim 1-10 any one of them is quickly from the preparation method for water-soluble liquid rubber plug of degrading, it is characterised in that： The preparation method be under the stirring condition of rotating speed 4000-5000r/min, sequentially add water, thickening agent, crosslinking accelerator, Crosslinking agent, rubber plug degradation agent, rubber plug degradation of promoter, solidification intensifier, are added while stirring, are further continued for stirring after addition 3-5min is spare.
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| CN113088271A (en) * | 2021-04-09 | 2021-07-09 | 中国石油天然气股份有限公司 | Sulfur-resistant liquid rubber plug and preparation method thereof |
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