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CN108841366A - High-temperature leakage-proof plugging agent and preparation method and application thereof - Google Patents

High-temperature leakage-proof plugging agent and preparation method and application thereof Download PDF

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Publication number
CN108841366A
CN108841366A CN201810605631.4A CN201810605631A CN108841366A CN 108841366 A CN108841366 A CN 108841366A CN 201810605631 A CN201810605631 A CN 201810605631A CN 108841366 A CN108841366 A CN 108841366A
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China
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sealing agent
high temperature
preparation
pressure
sealing
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CN201810605631.4A
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CN108841366B (en
Inventor
任从军
刘万海
常鹏梅
刘武友
聂凤云
王俊良
赵金姝
李佳
刘聪
张贺
张德友
李文杰
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Petrochina Co Ltd
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Petrochina Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K8/00Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
    • C09K8/42Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells
    • C09K8/46Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells containing inorganic binders, e.g. Portland cement
    • C09K8/467Compositions 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
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K8/00Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
    • C09K8/42Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells
    • C09K8/426Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells for plugging
    • EFIXED CONSTRUCTIONS
    • E21EARTH OR ROCK DRILLING; MINING
    • E21BEARTH OR ROCK DRILLING; OBTAINING OIL, GAS, WATER, SOLUBLE OR MELTABLE MATERIALS OR A SLURRY OF MINERALS FROM WELLS
    • E21B33/00Sealing or packing boreholes or wells
    • E21B33/10Sealing or packing boreholes or wells in the borehole
    • E21B33/13Methods or devices for cementing, for plugging holes, crevices or the like

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  • Life Sciences & Earth Sciences (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Geology (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Mining & Mineral Resources (AREA)
  • Inorganic Chemistry (AREA)
  • Fluid Mechanics (AREA)
  • Environmental & Geological Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Sealing Material Composition (AREA)

Abstract

The invention provides a high-temperature leakage-proof plugging agent and a preparation method and application thereof. The blocking agent comprises, by mass, 100% of ultrafine cement 40-60%, graphite particles 10-15%, silicon powder 10-15%, sodium tannate 1-3%, and the balance of water. The preparation method of the high-temperature leakage-proof plugging agent is simple and convenient, and the raw materials are easy to obtain; the prepared plugging agent has good temperature resistance, high pressure resistance, high breakthrough pressure resistance, good leakage resistance and high plugging capacity strength, and can be applied to the sealing and channeling sealing process technology of the high-temperature and high-pressure leakage well of the oil field to realize the sealing and channeling sealing of the high-temperature and high-pressure leakage serious well.

Description

A kind of high temperature lost circulation prevention sealing agent and its preparation method and application
Technical field
The invention belongs to oil well blocking technology field, it is related to a kind of high temperature lost circulation prevention sealing agent and preparation method thereof and answers With.
Background technique
Viscous crude mainly uses steam soak and steam flooding technology, exploitation the middle and later periods, due to more rounds steam soak and Prolonged steam drives, so that stratum steam forms the has channeling of fingering and ground interlayer;The casing of oil well is damaged and is missed;Outside casing Cementing concrete fails that formation pipe is outer to alter because prolonged high temperature and pressure corrodes, in this way, the high temperature and high pressure steam of injection may be taken With the natural gas and H in oil well2S gas alters channel and casing loses leak source and scurries out ground by the way that pipe is outer, generate explosion or It makes one to be poisoned, if foring ground large area gas leakage, would have to shut down some producing wells, it could even be possible to shutting down part area Block, this not only causes to seriously endanger to personal safety and environmental pollution, also causes and seriously affects to thickened oil recovery production, because This, it is necessary to sealing is implemented to these absorption wells, envelope is altered, shut-in well measure carries out comprehensive treatment.
Summary of the invention
It is altered outside for oil well leakage, oil gas under thickened oil recovery process high temperature in the prior art, difficult the problems such as blocking, this hair It is bright to be designed to provide a kind of high temperature lost circulation prevention sealing agent and preparation method thereof;The sealing agent preparation method is simple, and raw material is easy , the sealing agent viscosity being prepared is lower, is easy to stabilization in pump barrel, high temperature resistant, anti-high pressure.The present invention also aims to mention For application of the sealing agent in the pit shaft high temperature lost circulation prevention of oil field, it is applied in the pit shaft high temperature lost circulation prevention of oil field, lost circulation prevention Property good, high temperature resistant, anti-high pressure, have high breakthrough pressure, the needs of high temperature and pressure absorption well can be met.
The purpose of the present invention is achieved by the following technical programs:
On the one hand, the present invention provides a kind of high temperature lost circulation prevention sealing agent, by the sealing agent mass percent be 100% in terms of, Including:
In above-mentioned sealing agent, it is preferable that the superfine cement is G grades of oil-well cements.
In above-mentioned sealing agent, it is preferable that G grade specific surface area >=7000cm of the superfine cement2/g。
In above-mentioned sealing agent, G grades of oil-well cements are one of the main component of high temperature absorption well sealing agent, G grades of specific surfaces Product >=7000cm2/ g has good dissolubility suitable for the grouting of general fine spatial in water, and main function is conduct The principal element of the main closure of high temperature absorption well.
In above-mentioned sealing agent, it is preferable that the granularity of the graphite particle is 0.2-10mm.
In above-mentioned sealing agent, graphite particle is one of the main component of high temperature lost circulation prevention sealing agent, and graphite particle size is 0.2-10mm, it is not soluble in water, main function be in high temperature lost circulation prevention sealing agent as the High Temperature Plugging Agent of lost circulation prevention it is main because Element.
In above-mentioned sealing agent, silicon powder loses one of the packing material of sealing agent as high temperature resistant leak-proof, acts on for mentioning The temperature tolerance of sealing agent under high temperature.
In above-mentioned sealing agent, tannic acid sodium loses one of the packing material of sealing agent as high temperature resistant leak-proof, has in water Good dissolubility, wherein the deferred action for sealing agent under high temperature.
Superfine cement, graphite particle, four kinds of sealing agents of silicon powder and tannic acid sodium ingredient between be synergistic effect;Ultra-fine water The intensity for enhancing sealing agent under high temperature is played in mud, silicon powder and the effect of tannic acid sodium, and graphite particle is for leakage property below high temperature; If removing superfine cement in the high temperature lost circulation prevention sealing agent, only when silicon powder, tannic acid sodium and graphite particle, rise at high temperature not To the effect of shut-off capacity, there can be no solidification phenomenons in stratum;If it is graphite particle that the High Temperature Plugging Agent, which is removed, for high temperature Miss serious well no matter be pumped into stratum closure dosage number all not enough, formation leakage is still very serious, subsequent high temperature well Sealing, plugging technology cannot achieve.
In above-mentioned sealing agent, it is preferable that the density of the sealing agent is 1.85g/cm3-1.90g/cm3
On the other hand, the present invention also provides the preparation methods of above-mentioned sealing agent comprising following steps:
Water is stirred into swirl shape in advance, sequentially adds superfine cement, silicon powder, tannic acid sodium and graphite particle, when addition Room temperature stirs at low speed, and high-speed stirred after the completion of addition obtains the sealing agent.
In above-mentioned preparation method, it is preferable that the revolving speed stirred at low speed is that 2500 turns/min-3000 turns/min.
In above-mentioned preparation method, it is preferable that the revolving speed of high-speed stirred is that 7000 turns/min-7500 turns/min.
In above-mentioned preparation method, it is preferable that the time of high-speed stirred is 1min-2min.
Technology is altered in oil field high temperature and pressure absorption well sealing, envelope in another aspect, the present invention also provides above-mentioned sealing agents In application.
In above-mentioned application, it is preferable that the application the specific steps are:
The sealing agent prepared will be stirred in advance, test density reaches 1.85g/cm3-1.90g/cm3, disposable to inject In stratum, completes to block high temperature and pressure absorption well, seals the closure for altering technique.
In above-mentioned application, it is preferable that high temperature range is 200-300 DEG C;High pressure range is 5MPa-10MPa.
The preparation method of high temperature lost circulation prevention sealing agent of the invention is easy, and raw material is easy to get;The sealing agent heatproof being prepared Performance is good, high temperature resistant, anti-high pressure, has high breakthrough pressure, and lost circulation prevention is good, shut-off capacity intensity is high, is applied to oil Field high temperature and pressure absorption well sealing, envelope are altered in technology, be can be realized and are missed the sealing of serious well to high temperature and pressure, envelope is altered It blocks.
Specific embodiment
In order to which technical characteristic of the invention, purpose and beneficial effect are more clearly understood, now to skill of the invention Art scheme carries out described further below, but should not be understood as that limiting the scope of the invention.
Embodiment 1
The present embodiment provides a kind of high temperature lost circulation prevention sealing agent, it is in terms of 100% by the sealing agent mass percent, including:
Superfine cement is G grades of oil-well cements, G grades of specific surface area >=7000cm2/g;The granularity of graphite particle is 0.2- 0.6mm。
The present embodiment also provides the preparation method of the high temperature lost circulation prevention sealing agent, specially:Scene is stirred in advance with water At swirl shape, superfine cement, silicon powder and tannic acid sodium are sequentially added, is eventually adding graphite particle, room temperature low speed (2500 when addition Turn/min-3000 turns/min) stirring, high speed (7000 turns/min-7500 turns/min) stirring 1min-2min, is obtained after the completion of being added Obtain the sealing agent.The density of the sealing agent is 1.89g/cm3
Embodiment 2
The present embodiment provides a kind of high temperature lost circulation prevention sealing agent, it is in terms of 100% by the sealing agent mass percent, including:
Superfine cement is G grades of oil-well cements, G grades of specific surface area >=7000cm2/g;The granularity of graphite particle is 0.2-6mm.
The present embodiment also provides the preparation method of the high temperature lost circulation prevention sealing agent, specially:Scene is stirred in advance with water At swirl shape, superfine cement, silicon powder and tannic acid sodium are sequentially added, is eventually adding graphite particle, room temperature low speed (2500 when addition Turn/min-3000 turns/min) stirring, high speed (7000 turns/min-7500 turns/min) stirring 1min-2min, is obtained after the completion of being added Obtain the sealing agent.The density of the sealing agent is 1.89g/cm3
Embodiment 3
The present embodiment provides a kind of high temperature lost circulation prevention sealing agent, it is in terms of 100% by the sealing agent mass percent, including:
Superfine cement is G grades of oil-well cements, G grades of specific surface area >=7000cm2/g;The granularity of graphite particle is 0.2-6mm.
The present embodiment also provides the preparation method of the high temperature lost circulation prevention sealing agent, specially:Scene is stirred in advance with water At swirl shape, superfine cement, silicon powder and tannic acid sodium are sequentially added, is eventually adding graphite particle, room temperature low speed (2500 when addition Turn/min-3000 turns/min) stirring, high speed (7000 turns/min-7500 turns/min) stirring 1min-2min, is obtained after the completion of being added Obtain the sealing agent.The density of the sealing agent is 1.89g/cm3
Embodiment 4
The present embodiment provides a kind of high temperature lost circulation prevention sealing agent, it is in terms of 100% by the sealing agent mass percent, including:
Superfine cement is G grades of oil-well cements, G grades of specific surface area >=7000cm2/g;The granularity of graphite particle is 0.2- 10mm。
The present embodiment also provides the preparation method of the high temperature lost circulation prevention sealing agent, specially:Scene is stirred in advance with water At swirl shape, superfine cement, silicon powder and tannic acid sodium are sequentially added, is eventually adding graphite particle, room temperature low speed (2500 when addition Turn/min-3000 turns/min) stirring, high speed (7000 turns/min-7500 turns/min) stirring 1min-2min, is obtained after the completion of being added Obtain the sealing agent.The density of the sealing agent is 1.89g/cm3
Cure test
High temperature lost circulation prevention sealing agent prepared by above-described embodiment 1-4 carries out indoor high temperature phase change modeling experiment, surveys Curing time is tried, experimental result is shown in Table 1.
Table 1:
From 1 experimental data of table:Under different mass concentrations, high temperature lost circulation prevention sealing agent pumps in high temperature pit shaft Time, it is as the upper limit, therefore by changing sealing agent that the time, which is less than sealing agent under hot conditions not occur dodging the solidifying time, The ratio of each raw material can grasp the pump time of safest high temperature lost circulation prevention sealing agent.
High temperature resistant experiment
Sample test block is made after sealing agent is solidified, is put into high-temperature high-pressure reaction kettle, places into clear water for sample test block It floods, by the application method of high-pressure bottle, sample test block is subjected to the experiment of 1d-7d heatproof under the conditions of 300 DEG C -350 DEG C.Heatproof After experiment, sample test block, compression strength of the test sample test block after heatproof experiment are taken out, and compare sample examination before heatproof The compression strength of block, experimental result are shown in Table 2.
Table 2:
From 2 experimental data of table:By changing the ratio of the raw material of sealing agent, can control pressure is 7.8- 10.2MPa controls the pressure of high temperature lost circulation prevention sealing agent, can satisfy the plugging strength requirement of different measure well.
Sealing ratiod and breakthrough pressure
High temperature lost circulation prevention sealing agent prepared by embodiment 1-4 carries out laboratory core simulated experiment, measures the gap of rock core Volume PV and core permeability K0.Reinject the sealing agent of 10PV or more.Under the conditions of 90 DEG C, Hou Ning is for 24 hours.Hou Ning terminates, At room temperature, core permeability K after blocking is surveyed1, continue the rated pressure that device is boosted to 0.1MPa/min hereinafter, if after blocking Rock core flow out the first drop of liquid pressure be breakthrough pressure.And sealing ratiod and breakthrough pressure gradient are calculated separately as the following formula.
η-sealing ratiod indicates (%) with percentage;
K0Permeability before reservoir core plugging, (10-3 μm of unit millidarcy2);
K1Permeability after reservoir core plugging, (10-3 μm of unit millidarcy2);
L- rock core length.
Sealing ratiod and breakthrough pressure after closure, test result are shown in Table 3.
Table 3:
From 3 experimental data of table:The sealing agent sealing ratiod of the embodiment of the present invention can reach 100%, and breakthrough pressure reaches To 75MPa or more, the plugging strength requirement of different measure well can satisfy.
Embodiment 5
The present embodiment provides the high temperature lost circulation prevention sealing agents of the preparation of embodiment 3 in oil field high temperature and pressure absorption well sealing, envelope Alter the application in technology.
Du84-50-148Jing is steam injection well, and well depth 715m, steam injection string pen tip is between the oil reservoir upper bound and lower bound, shaft bottom Well temperature is up to 242 DEG C, tubing pressure 5MPa, casing pressure 2.5MPa, belongs to lifting well head, pit shaft is by the entire pit shaft in the shaft bottom 110m- Temperature again 200 DEG C -250 DEG C or so fluctuation, well head to bottom pressure 5MPa or so fluctuate, therefore shaft bottom leakage seriously.
The high temperature lost circulation prevention sealing agent is indoors under conditions of 240 DEG C, cure test 1.5h, for 600m's or so High temperature pit shaft, high temperature lost circulation prevention sealing agent safe can be pumped into stratum in pit shaft, under 350 DEG C of hot conditions, envelope The pressure of blocking agent can achieve 8.8MPa.Using this formula, lost circulation prevention 30m is increased temperature in the field3, stir, match Density at sealing agent is 1.89g/cm3.Observation casing pressure variation during squeezing is instead squeezed fresh water balance and is squeezed when casing pressure rises very fast Grey pressure.It has infused high temperature lost circulation prevention sealing agent and has just pushed up clear water 2.4m again3, upper lifting pipe post 1m-2m, until clear water is shown in backwash, wash-off Extra high temperature lost circulation prevention sealing agent.It waits and coagulates 24 hours, to well section pressure testing 15MPa, 30 minutes pressure drop≤0.5Mpa is blocked, block It works well.
In conclusion the preparation method of high temperature lost circulation prevention sealing agent of the invention is easy, raw material is easy to get;The envelope being prepared Blocking agent heat resistance is good, high temperature resistant, anti-high pressure, has high breakthrough pressure, and lost circulation prevention is good, shut-off capacity intensity is high, by it It is altered in technology applied to oil field high temperature and pressure absorption well sealing, envelope, can be realized the envelope for missing serious well to high temperature and pressure The closure that layer, envelope are altered.

Claims (10)

1. a kind of high temperature lost circulation prevention sealing agent, which is characterized in that by the sealing agent mass percent be 100% in terms of, including:
2. sealing agent according to claim 1, it is characterised in that:The superfine cement is G grades of oil-well cements.
3. sealing agent according to claim 2, it is characterised in that:G grade specific surface area >=7000cm of the superfine cement2/ g。
4. sealing agent according to claim 1, it is characterised in that:The granularity of the graphite particle is 0.2-10mm.
5. sealing agent according to claim 1-4, it is characterised in that:The density of the sealing agent is 1.85g/cm3- 1.90g/cm3
6. the preparation method of any one of the claim 1-5 sealing agent comprising following steps:
Water is stirred into swirl shape in advance, sequentially adds superfine cement, silicon powder, tannic acid sodium and graphite particle, room temperature when addition It stirs at low speed, high-speed stirred after the completion of addition obtains the sealing agent.
7. preparation method according to claim 6, it is characterised in that:
The revolving speed stirred at low speed is that 2500 turns/min-3000 turns/min;
Preferably, the revolving speed of high-speed stirred is that 7000 turns/min-7500 turns/min.
8. preparation method according to claim 6, it is characterised in that:The time of high-speed stirred is 1min-2min.
9. any one of the claim 1-5 sealing agent alters answering in technology in oil field high temperature and pressure absorption well sealing, envelope With.
10. application according to claim 9, which is characterized in that it is described application the specific steps are:
The sealing agent prepared will be stirred in advance, test density reaches 1.85g/cm3-1.90g/cm3, disposably inject stratum In, it completes to block high temperature and pressure absorption well, seal the closure for altering technique;
Preferably, high temperature range is 200-300 DEG C;High pressure range is 5MPa-10MPa.
CN201810605631.4A 2018-06-13 2018-06-13 High-temperature leakage-proof plugging agent and preparation method and application thereof Active CN108841366B (en)

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CN111188606A (en) * 2020-01-14 2020-05-22 中国石油大学(华东) Low-temperature expandable graphite for steam injection channeling sealing of heavy oil reservoir and preparation method and application thereof
CN111663935A (en) * 2019-03-08 2020-09-15 中石化石油工程技术服务有限公司 Method and system for evaluating shaft annulus air tightness
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CN113234424A (en) * 2021-05-20 2021-08-10 嘉华特种水泥股份有限公司 Low-density well cementation cement slurry system suitable for medium-high temperature stratum and preparation method thereof
CN114635680A (en) * 2022-03-08 2022-06-17 中国石油大学(北京) System and method for determining butt seam high control capability of artificial partition plate

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CN111663935A (en) * 2019-03-08 2020-09-15 中石化石油工程技术服务有限公司 Method and system for evaluating shaft annulus air tightness
CN111663935B (en) * 2019-03-08 2023-05-26 中石化石油工程技术服务有限公司 Method and system for evaluating annular air tightness of shaft
CN111188606A (en) * 2020-01-14 2020-05-22 中国石油大学(华东) Low-temperature expandable graphite for steam injection channeling sealing of heavy oil reservoir and preparation method and application thereof
CN112647895A (en) * 2020-12-28 2021-04-13 黑龙江弘力通能源技术服务有限公司 Method for plugging leakage of oil-gas well casing by adopting liquid casing
CN113234424A (en) * 2021-05-20 2021-08-10 嘉华特种水泥股份有限公司 Low-density well cementation cement slurry system suitable for medium-high temperature stratum and preparation method thereof
CN113234424B (en) * 2021-05-20 2022-08-19 嘉华特种水泥股份有限公司 Low-density well cementation cement slurry system suitable for medium-high temperature stratum and preparation method thereof
CN114635680A (en) * 2022-03-08 2022-06-17 中国石油大学(北京) System and method for determining butt seam high control capability of artificial partition plate

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