CN106867485B - High-temperature-resistant plugging agent, preparation method and application thereof - Google Patents
High-temperature-resistant plugging agent, preparation method and application thereof Download PDFInfo
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- CN106867485B CN106867485B CN201510916310.2A CN201510916310A CN106867485B CN 106867485 B CN106867485 B CN 106867485B CN 201510916310 A CN201510916310 A CN 201510916310A CN 106867485 B CN106867485 B CN 106867485B
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- polyacrylamide
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- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 183
- 238000007789 sealing Methods 0.000 claims abstract description 163
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 53
- 229920002401 polyacrylamide Polymers 0.000 claims abstract description 36
- 239000002245 particle Substances 0.000 claims abstract description 34
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical class [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims abstract description 23
- 230000008961 swelling Effects 0.000 claims description 30
- 239000003002 pH adjusting agent Substances 0.000 claims description 18
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 9
- 229920000642 polymer Polymers 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 7
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 3
- 239000000908 ammonium hydroxide Substances 0.000 claims description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims 1
- 238000004090 dissolution Methods 0.000 claims 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical group [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims 1
- 238000006116 polymerization reaction Methods 0.000 claims 1
- 229910052708 sodium Inorganic materials 0.000 claims 1
- 239000011734 sodium Substances 0.000 claims 1
- 230000015572 biosynthetic process Effects 0.000 abstract description 12
- 238000005553 drilling Methods 0.000 abstract description 12
- 238000010276 construction Methods 0.000 abstract description 8
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 abstract description 3
- 235000010299 hexamethylene tetramine Nutrition 0.000 abstract description 2
- 229960004011 methenamine Drugs 0.000 abstract description 2
- 239000003208 petroleum Substances 0.000 abstract description 2
- 239000004312 hexamethylene tetramine Substances 0.000 abstract 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 36
- 238000006243 chemical reaction Methods 0.000 description 24
- 238000004132 cross linking Methods 0.000 description 23
- 239000000084 colloidal system Substances 0.000 description 18
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 12
- 229920003023 plastic Polymers 0.000 description 10
- 239000000126 substance Substances 0.000 description 9
- 230000000694 effects Effects 0.000 description 7
- 239000011148 porous material Substances 0.000 description 7
- 239000012530 fluid Substances 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 239000003513 alkali Substances 0.000 description 2
- 125000003368 amide group Chemical group 0.000 description 2
- 150000001412 amines Chemical class 0.000 description 2
- 230000000903 blocking effect Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000003431 cross linking reagent Substances 0.000 description 2
- 239000003292 glue Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000013618 particulate matter Substances 0.000 description 2
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 description 1
- -1 Acrylamide solution;Sulfonated phenol formaldehyde resin Chemical class 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 239000013043 chemical agent Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- LCDFWRDNEPDQBV-UHFFFAOYSA-N formaldehyde;phenol;urea Chemical class O=C.NC(N)=O.OC1=CC=CC=C1 LCDFWRDNEPDQBV-UHFFFAOYSA-N 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 229920005610 lignin Polymers 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- VIKNJXKGJWUCNN-XGXHKTLJSA-N norethisterone Chemical compound O=C1CC[C@@H]2[C@H]3CC[C@](C)([C@](CC4)(O)C#C)[C@@H]4[C@@H]3CCC2=C1 VIKNJXKGJWUCNN-XGXHKTLJSA-N 0.000 description 1
- 239000003129 oil well Substances 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 229920000867 polyelectrolyte Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 238000006277 sulfonation reaction Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 230000008719 thickening Effects 0.000 description 1
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
- C09K8/426—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells for plugging
-
- 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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- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Sealing Material Composition (AREA)
Abstract
The invention discloses a high-temperature-resistant plugging agent, a preparation method and application thereof, and belongs to the technical field of petroleum drilling plugging. The high-temperature resistant plugging agent comprises the following components in percentage by mass: 2% -3% of polyacrylamide; 1% -2% of sulfonated phenolic resin; 0.9 to 2 percent of hexamethylene tetramine; 3% -5% of water-swelling type particle plugging agent; 2% -6% of a unidirectional pressure sealing agent; 0-3% of an alkaline pH regulator; water and the balance. The plugging agent has good high-temperature resistance, and can meet the plugging requirement of drilling at 80-150 ℃. Meanwhile, the plugging agent has lower viscosity and fluidity before gel formation, so that plugging construction is facilitated; the gel has higher strength and stability after being formed, and has good plugging performance.
Description
Technical field
The present invention relates to oil drilling leakage stopping technology field, in particular to a kind of sealing agent resistant to high temperatures, preparation method and its
Using.
Background technique
In Process of Oil Well Drilling, leakage phenomenon often occurs, i.e., drilling fluid leaks into formation pore, crack in pit shaft
Phenomenon.Leakage is very harmful to drillng operation, will lead to loss of drilling fluid, drilling period extend, can also cause chip off-falling, bit freezing,
The accidents such as hole collapse.Therefore, it in order to guarantee being normally carried out for drillng operation, needs using sealing agent to the stratum that leakage occurs
It is blocked.
Currently used sealing agent mainly includes physics sealing agent and chemical leak-stopping agent.Physics sealing agent is solid particulate matter
Matter.The principle of leak stopping is carried out using physics sealing agent are as follows: according to formation pore, the size in crack, select the physics of corresponding partial size
Sealing agent blocks the hole on stratum, crack.Chemical leak-stopping agent mainly includes cement, resin etc..Using chemical leak-stopping agent
Carry out the principle of leak stopping are as follows: chemical leak-stopping agent enters after formation pore, crack, crosslinks reaction under certain condition and generates
Plural gel substance is to block the hole on stratum, crack.Compared with physics sealing agent, chemical leak-stopping agent can be certainly
Dynamic to adapt to various sizes of formation pore, crack, plugging effect is more preferable.
In the implementation of the present invention, the inventors discovered that in the prior art the prior art has at least the following problems: existingization
It is poor to learn sealing agent high temperature resistant property, it cannot ground-to-ground the hole of layer, crack be blocked very well when formation temperature is higher.
Summary of the invention
In order to solve the above technical problems, the present invention provides a kind of sealing agent resistant to high temperatures, preparation method and applications.
Specifically, including technical solution below:
First aspect present invention provides a kind of sealing agent resistant to high temperatures, and the sealing agent resistant to high temperatures includes following mass percent
Component:
Polyacrylamide, 2%~3%；
Sulfonated phenol formaldehyde resin, 1%~2%；
Hexa, 0.9%~2%；
Water swelling type particle sealing agent, 3%~5%；
Uniaxial pressure sealer, 2%~6%；
Alkaline pH adjusting agent, 0~3%；
Water, surplus.
Preferably, the alkaline pH adjusting agent is selected from least one of sodium hydroxide, potassium hydroxide and ammonium hydroxide.
Preferably, the mass percent of the alkaline pH adjusting agent is 0.5%~2%.
Preferably, the mass percent of the hexa is 1%~2%.
Preferably, the mass percent of the uniaxial pressure sealer is 3%~5%.
Preferably, the number-average molecular weight of the polyacrylamide is 3,000,000~5,000,000.
Preferably, the partial size of the water swelling type particle sealing agent is 1.2 millimeters hereinafter, the water swelling type particle
The expansion multiple of sealing agent is 3 times or more.
Preferably, the partial size of the uniaxial pressure sealer is 0.28 millimeter or less.
Second aspect of the present invention provides a kind of preparation method of the sealing agent resistant to high temperatures of first aspect present invention, the preparation
Method the following steps are included:
Polyacrylamide is dissolved in the water to obtain polyacrylamide solution by step a；
Sulfonated phenol formaldehyde resin and hexa are added in the polyacrylamide solution by step b, and stirring is extremely
Polymer solution is obtained after being completely dissolved；
Alkaline pH adjusting agent, water swelling type particle sealing agent and uniaxial pressure sealer are added to described by step c
In polymer solution, stirring is to after being completely dissolved up to the sealing agent resistant to high temperatures.
Third aspect present invention provides a kind of application of the sealing agent resistant to high temperatures of first aspect present invention, i.e., by the anti-height
Warm sealing agent is delivered to the stratum missed, and makes the sealing agent resistant to high temperatures at stratum standing 6 hours or more；It is described
The formation temperature on stratum is 80~150 DEG C.
The beneficial effect of technical solution provided in an embodiment of the present invention is:
In sealing agent provided in an embodiment of the present invention, all containing work in polyacrylamide amine molecule and sulfonated phenol formaldehyde resin molecule
Property reactive group, can crosslink reaction and form gel, to block to the hole on stratum, crack.Wherein sulphonated phenol
Urea formaldehyde has good high temperature resistant property, can be improved the high temperature resistant property of sealing agent entirety.Meanwhile the water suction in sealing agent
Intumescent particle sealing agent and uniaxial pressure sealer also have performance resistant to high temperatures, are also beneficial to improve sealing agent entirety
High temperature resistant property.Therefore, sealing agent provided in an embodiment of the present invention has good high temperature resistant property, can satisfy 80~150
The leak stopping of DEG C drilling well needs.In addition, sealing agent provided in an embodiment of the present invention has good stream before being cross-linked to form colloid
Dynamic performance, convenient for construction；The colloid intensity with higher formed after crosslinking, is able to bear the pressure of 8MPa or more, and
Stability is good, its performance can be stably kept 70 days or more in the high temperature environment.
Specific embodiment
To keep technical solution of the present invention and advantage clearer, embodiment of the present invention is made below further detailed
Description.
First aspect present invention provides a kind of sealing agent resistant to high temperatures, which includes following mass percent
Component:
Polyacrylamide, 2%~3%；
Sulfonated phenol formaldehyde resin, 1%~2%；
Hexa, 0.9%~2%；
Water swelling type particle sealing agent, 3%~5%；
Uniaxial pressure sealer, 2%~6%；
Alkaline pH adjusting agent, 0~3%；
Water, surplus.
The embodiment of the present invention is provided to be optimized by composition to sealing agent and proportion, and having obtained one kind has
The sealing agent of good high temperature resistant property.In the sealing agent:
(1), polyacrylamide is water soluble organic polymer polymer, the amido (- NH on strand side chain2) can
Reaction is crosslinked with crosslinking agent and generates gel, and the hole on stratum and crack are blocked.In addition, polyacrylamide is in neutral and alkali
Property medium in show the feature of high polymeric polyelectrolyte, there is thickening and flocculated effect, additionally it is possible to reduce the mill between liquid
Wipe resistance, improve sealing agent gel before mobility, convenient for blocking construction (referring to: Wang Zhonghua etc. writes, " oil field chemical
Application manual ", Sinopec publishing house, 160-161, page 286,338).
(2), sulfonated phenol formaldehyde resin is obtained by the phenol and formaldehyde condensation polymer of sulfonation, the hydroxyl in molecule can and polyacrylamide
Amido in amine molecule reacts to form gel.Meanwhile sulfonated phenol formaldehyde resin has good high temperature resistant property, can be improved
The high temperature resistant property of sealing agent, additionally it is possible to improve the stability of sealing agent, improve the viscoplasticity of colloid after gel, enhancing colloid is attached
Wall ability (referring to: Zhao Fulin writes, " chemical agent for oil recovery ", publishing house, University of Petroleum, publishes within 1997, the 39-42 pages).
(3), water swelling type particle sealing agent be solid particulate matter and organic macromolecule compound, be khaki or
Light gray solid particle, not soluble in water, water-swellable.In the embodiment of the present invention, water swelling type particle sealing agent is used to improve
The concentration of sealing agent and the gel strength after gel block big hole and crack, prevent the liquid component in sealing agent from existing
Be lost before gel, guarantee sealing agent plugging effect (referring to: Wang Zhonghua etc. writes, " oil field chemical application manual ", China
Petrochemical industry publishing house, page 287).In addition, water swelling type particle sealing agent also has performance resistant to high temperatures, it is also beneficial to improve
The high temperature resistant property of sealing agent.
(4), uniaxial pressure sealer, also known as drill-feeding plugging agent are answered by the cellulose powder of different-grain diameter, lignin powder
With forming, standard Q/SY 1096-2012 is executed.Uniaxial pressure sealer usually adds in drilling fluid, penetrates into ground with drilling fluid
Layer, under the effect of stratum uniaxial pressure difference, block formation pore and crack (referring to: Wang Zhonghua etc. writes, and " oil field chemical is real
With handbook ", Sinopec publishing house, the 159-160 pages).In sealing agent provided in an embodiment of the present invention, uniaxial pressure closing
The effect of agent mainly prevents liquid component in sealing agent to be lost, and guarantees the plugging effect of sealing agent.
(5), hexa also known as methenamine decompose in alkaline hot environment and generate formaldehyde, formaldehyde can with it is poly-
Acrylamide and sulfonated phenol formaldehyde resin react.Therefore, hexa is in sealing agent provided in an embodiment of the present invention
As auxiliary crosslinking agent, gel strength is improved.
(6), alkaline pH adjusting agent generates formaldehyde since hexa just decomposes in alkaline environment, and formaldehyde
Amount will affect the time of sealing agent gel, therefore, the gel time and plugging agent system of sealing agent provided in an embodiment of the present invention
PH value it is related.The gel time of sealing agent can be adjusted by the pH value that alkaline pH adjuster adjusts sealing agent,
Make sealing agent that there is good mobility before reaching target position, set apart for blocking construction, convenient for construction；And when stifled
Leak agent reach target position after, can rapid gel, formation pore and crack are blocked.
By the mutual cooperation between above-mentioned grouping point, synergistic effect, sealing agent provided in an embodiment of the present invention has good
Good high temperature resistant property, can satisfy the leak stopping needs of 80~150 DEG C of drilling wells.And sealing agent provided in an embodiment of the present invention is solidifying
The colloid intensity with higher formed after glue, is able to bear the pressure of 8MPa or more, and stability is good, in hot environment
In its its performance can stably keep 70 days or more.
In above-mentioned sealing agent resistant to high temperatures, one in the preferred sodium hydroxide of alkaline pH adjusting agent, potassium hydroxide or ammonium hydroxide
Kind or several compounds.Wherein more preferable sodium hydroxide because sodium hydroxide is cheap, can reduce sealing agent at
This.
In above-mentioned sealing agent resistant to high temperatures, the mass percent of alkaline pH adjusting agent should be according to the temperature of underground and solidifying
The glue time needs to be arranged.When temperature when underground is higher, it can suitably reduce the amount of alkaline pH adjusting agent or not add alkali
Property pH adjusting agent, because the gel time of sealing agent is inherently shorter when temperature is higher, if the matter of alkaline pH adjusting agent
Measure the relatively high gel time for making sealing agent of percentage it is too short if, sealing agent reach target position before will gel, flowing
Property be deteriorated, cause equipment to block.Similarly, when downhole temperature is lower, it can suitably increase the amount of alkaline pH adjusting agent, make leak stopping
Agent reaches energy PhastGel behind target position, improves construction efficiency.The more satisfactory gel time of sealing agent are as follows: when sealing agent reaches
To after target position, cross-linking reaction takes place within 0.5~1 hour, 6~10 hours gel strengths reach maximum.Alkaline pH is adjusted
The mass percent of agent preferably 0.5%~2%, can for 0.6%, 0.7%, 0.8%, 0.9%, 1.0%, 1.1%, 1.2%,
1.3%, 1.4%, 1.5%, 1.6%, 1.7%, 1.8%, 1.9% etc..
In above-mentioned sealing agent resistant to high temperatures, the mass percent of polyacrylamide can for 2.1%, 2.2%, 2.3%,
2.4%, 2.5%, 2.6%, 2.7%, 2.8%, 2.9% etc..
In above-mentioned sealing agent resistant to high temperatures, the mass percent of sulfonated phenol formaldehyde resin can for 1.1%, 1.2%,
1.3%, 1.4%, 1.5%, 1.6%, 1.7%, 1.8%, 1.9% etc..
In above-mentioned sealing agent resistant to high temperatures, the mass percent of hexa preferably 1%~2%, Ke Yiwei
1.1%, 1.2%, 1.3%, 1.4%, 1.5%, 1.6%, 1.7%, 1.8%, 1.9% etc.
In above-mentioned sealing agent resistant to high temperatures, the mass percent of water swelling type particle sealing agent can for 3.2%,
3.4%, 3.6%, 3.8%, 4.0%, 4.2%, 4.4%, 4.6%, 4.8% etc..
In above-mentioned sealing agent resistant to high temperatures, the mass percent of uniaxial pressure sealer preferably 3%~5%, Ke Yiwei
3.2%, 3.4%, 3.6%, 3.8%, 4.0%, 4.2%, 4.4%, 4.6%, 4.8% etc..
In above-mentioned sealing agent resistant to high temperatures, the number-average molecular weight of polyacrylamide is preferably 3,000,000~5,000,000.Such as
It can be 3,200,000,3,400,000,3,500,000,3,600,000,3,800,000,4,000,000,4,200,000,4,400,000,4,500,000,4,600,000,4,800,000 etc..Such as
The number-average molecular weight of fruit polyacrylamide is too small, and the colloid viscosity, intensity after making sealing agent gel are lower, cannot effectively block
Formation pore, crack；If the number-average molecular weight of polyacrylamide is excessive, dissolved mobility is deteriorated or does not flow
Dynamic property, causes finally to can not be successfully construction.
In above-mentioned sealing agent resistant to high temperatures, in order to divide water swelling type particle sealing agent uniformly in plugging agent system
It dissipates, the partial size of water swelling type particle sealing agent is preferably 1.2 millimeters hereinafter, can be for example 1 millimeter, 0.8 millimeter, 0.6 milli
Rice etc..Meanwhile volume expansion multiple is preferably 3 times or more after the water suction of water swelling type particle sealing agent.
It is single in order to keep uniaxial pressure sealer evenly dispersed in plugging agent system in above-mentioned sealing agent resistant to high temperatures
Partial size to pressure seal agent is preferably 0.28 millimeter hereinafter, for example can be 0.25 millimeter, 0.2 millimeter, 0.15 millimeter, 0.1
Millimeter etc..
In above-mentioned sealing agent resistant to high temperatures, the manufacturer of each component and model do not have particular/special requirement, as long as performance is joined
Number meets the requirement of the embodiment of the present invention.Wherein, the preferred Shandong De Shunyuan share of water swelling type particle sealing agent is limited
The GWS-1 type particle sealing agent of company's production, the DF-1 type of the preferred Henan Huixian development auxiliary reagent factory production of uniaxial pressure sealer
Uniaxial pressure sealer.
Sealing agent provided in an embodiment of the present invention can be prepared by the following method to obtain, which includes following step
It is rapid:
Step a is dissolved in the water the polyacrylamide to obtain polyacrylamide molten according to the formula of scheduled sealing agent
Liquid；
Sulfonated phenol formaldehyde resin and hexa are added in above-mentioned polyacrylamide solution by step b, and stirring is extremely
Polymer solution is obtained after being completely dissolved；
Alkaline pH adjusting agent, water swelling type particle sealing agent and uniaxial pressure sealer are added to above-mentioned by step c
In polymer solution, stirring is to after being completely dissolved up to the sealing agent resistant to high temperatures.
The application method of sealing agent provided in an embodiment of the present invention are as follows: pump truck is used after preparing sealing agent in ground tanks
It is delivered to the stratum missed.Sealing agent is delivered to behind target position to make sealing agent formation at target locations stand 6 hours with
On, make sufficiently to react between sealing agent each component, gel strength is made to reach maximum.Sealing agent will penetrate into one depthkeeping of formation at target locations
Degree, so that the elasticity for forming more firm around the borehole wall blocks band, to guarantee plugging effect.
Main agents used are as follows in following example 1~10:
Polyacrylamide, manufacturer: gloomy (China) the flocculant Co., Ltd of love, number-average molecular weight 3,000,000；
Sulfonated phenol formaldehyde resin, manufacturer: Tianjin runs quickly and splashes surface chemistry auxiliary reagent factory, model: GWO；
Water swelling type particle sealing agent, manufacturer: Shandong De Shunyuan limited liability company, model: GWS-1, partial size
1.2 millimeters, expansion multiple is 3 times or more after water suction；
Uniaxial pressure sealer, manufacturer: Henan Huixian development auxiliary reagent factory, model: DF-1,0.28 millimeter of partial size.
Embodiment 1:
The present embodiment provides a kind of sealing agent resistant to high temperatures, which is included the following components'mass percentage:
Polyacrylamide, 2%；
Sulfonated phenol formaldehyde resin, 1%；
Water swelling type particle sealing agent, 5%；
Hexa, 1%；
Uniaxial pressure sealer, 5%；
Sodium hydroxide, 0.5%；
Water, 85.5%.
The sealing agent resistant to high temperatures the preparation method comprises the following steps: according to said ratio, polyacrylamide is dissolved in the water and is gathered
Acrylamide solution；Sulfonated phenol formaldehyde resin and hexa are added in above-mentioned polyacrylamide solution, stirring is extremely
Polymer solution is obtained after being completely dissolved；Sodium hydroxide, water swelling type particle sealing agent and uniaxial pressure sealer are added
Enter into above-mentioned polymer solution, stirs to the sealing agent resistant to high temperatures for being completely dissolved rear the present embodiment to obtain the final product.
The crosslinking reaction may not occur at normal temperature for the sealing agent resistant to high temperatures, not plastic, and apparent viscosity at normal temperature is
121mPas stands 3 hours at 120 DEG C and cross-linking reaction takes place, and stands the gel strength that 8 hours form and reaches maximum, this
When colloid viscosity be 11732mPas, elasticity modulus 533Pa, viscous modulus 308Pa, 50 μm2Pressure-bearing after reservoir core plugging
For 9.2MPa.The performance of the sealing agent can be stably kept 70 days at 120 DEG C.
Embodiment 2
The present embodiment provides a kind of sealing agent resistant to high temperatures, which is included the following components'mass percentage:
Polyacrylamide, 2.5%；
Sulfonated phenol formaldehyde resin, 1.5%；
Water swelling type particle sealing agent, 3%；
Hexa, 1.5%；
Uniaxial pressure sealer, 3%；
Water, 88.5%.
The preparation method is the same as that of Example 1 for the sealing agent resistant to high temperatures.
The crosslinking reaction may not occur at normal temperature for the sealing agent resistant to high temperatures, not plastic, and apparent viscosity at normal temperature is
116mPas stands 3 hours at 120 DEG C and cross-linking reaction takes place, and stands the gel strength that 8 hours form and reaches maximum, this
When colloid viscosity be 80206mPas, elasticity modulus 543.2Pa, viscous modulus 104.1Pa, 50 μm2After reservoir core plugging
Pressure-bearing is 9.2MPa.The performance of the sealing agent can be stably kept 70 days at 120 DEG C.
Embodiment 3
The present embodiment provides a kind of sealing agent resistant to high temperatures, which is included the following components'mass percentage:
Polyacrylamide, 2%；
Sulfonated phenol formaldehyde resin, 1.2%；
Water swelling type particle sealing agent, 4%；
Hexa, 1.3%；
Uniaxial pressure sealer, 5%；
Sodium hydroxide, 0.3%；
Water, 86.2%.
The preparation method is the same as that of Example 1 for the sealing agent resistant to high temperatures.
The crosslinking reaction may not occur at normal temperature for the sealing agent resistant to high temperatures, not plastic, and apparent viscosity at normal temperature is
116mPas stands 3 hours at 120 DEG C and cross-linking reaction takes place, and stands the gel strength that 8 hours form and reaches maximum, this
When colloid viscosity be 78960mPas, elasticity modulus 559Pa, viscous modulus 354.9Pa, 10 μm2It is held after reservoir core plugging
Pressure is 12.4MPa.The performance of the sealing agent can be stably kept 70 days at 120 DEG C.
Embodiment 4
The present embodiment provides a kind of sealing agent resistant to high temperatures, which is included the following components'mass percentage:
Polyacrylamide, 2%；
Sulfonated phenol formaldehyde resin, 1.2%；
Water swelling type particle sealing agent, 3%；
Hexa, 1.3%；
Uniaxial pressure sealer, 6%；
Sodium hydroxide, 0.5%；
Water, 86%.
The preparation method is the same as that of Example 1 for the sealing agent resistant to high temperatures.
The crosslinking reaction may not occur at normal temperature for the sealing agent resistant to high temperatures, not plastic, and apparent viscosity at normal temperature is
115mPas stands 2 hours at 150 DEG C and cross-linking reaction takes place, and stands the gel strength that 8 hours form and reaches maximum, this
When colloid viscosity be 105400mPas, elasticity modulus 559Pa, viscous modulus 354.9Pa, 10 μm2After reservoir core plugging
Pressure-bearing is 12.2MPa.The performance of the sealing agent can be stably kept 70 days at 150 DEG C.
Embodiment 5
The present embodiment provides a kind of sealing agent resistant to high temperatures, which is included the following components'mass percentage:
Polyacrylamide, 3%；
Sulfonated phenol formaldehyde resin, 1.2%；
Water swelling type particle sealing agent, 5%；
Hexa, 1.2%；
Uniaxial pressure sealer, 2%；
Sodium hydroxide, 1%；
Water, 86.6%.
The preparation method is the same as that of Example 1 for the sealing agent resistant to high temperatures.
The crosslinking reaction may not occur at normal temperature for the sealing agent resistant to high temperatures, not plastic, and apparent viscosity at normal temperature is
118mPas stands 2 hours at 150 DEG C and cross-linking reaction takes place, and stands the gel strength that 8 hours form and reaches maximum, this
When colloid viscosity be 113809mPas, elasticity modulus 527Pa, viscous modulus 360Pa, 15 μm2It is held after reservoir core plugging
Pressure is 13.4MPa.The performance of the sealing agent can be stably kept 70 days at 150 DEG C.
Embodiment 6
The present embodiment provides a kind of sealing agent resistant to high temperatures, which is included the following components'mass percentage:
Polyacrylamide, 3%；
Sulfonated phenol formaldehyde resin, 4%；
Water swelling type particle sealing agent, 5%；
Hexa, 0.9%；
Uniaxial pressure sealer, 3%；
Water, 84.1%.
The preparation method is the same as that of Example 1 for the sealing agent resistant to high temperatures.
The crosslinking reaction may not occur at normal temperature for the sealing agent resistant to high temperatures, not plastic, and apparent viscosity at normal temperature is
149mPas stands 3 hours at 130 DEG C and cross-linking reaction takes place, and stands the gel strength that 8 hours form and reaches maximum, this
When colloid viscosity be 11591mPas, elasticity modulus 527.8Pa, viscous modulus 360Pa, 12 μm2It is held after reservoir core plugging
Pressure is 12.5MPa.The performance of the sealing agent can be stably kept 70 days at 130 DEG C.
Embodiment 7
The present embodiment provides a kind of sealing agent resistant to high temperatures, which is included the following components'mass percentage:
Polyacrylamide, 2.5%；
Sulfonated phenol formaldehyde resin, 1.2%；
Water swelling type particle sealing agent, 5%；
Hexa, 0.9%；
Uniaxial pressure sealer, 3%；
Sodium hydroxide, 0.5%；
Water, 86.9%.
The preparation method is the same as that of Example 1 for the sealing agent resistant to high temperatures.
The crosslinking reaction may not occur at normal temperature for the sealing agent resistant to high temperatures, not plastic, and apparent viscosity at normal temperature is
123mPas stands 3 hours at 130 DEG C and cross-linking reaction takes place, and stands the gel strength that 8 hours form and reaches maximum, this
When colloid viscosity be 100875mPas, elasticity modulus 479.3Pa, viscous modulus 215.7Pa, 20 μm2Reservoir core plugging
Pressure-bearing is 9.8MPa afterwards.The performance of the sealing agent can be stably kept 70 days at 130 DEG C.
Embodiment 8
The present embodiment provides a kind of sealing agent resistant to high temperatures, which is included the following components'mass percentage:
Polyacrylamide, 3%；
Sulfonated phenol formaldehyde resin, 1.5%；
Water swelling type particle sealing agent, 5%；
Hexa, 0.9%；
Uniaxial pressure sealer, 3%；
Water, 86.6%.
The preparation method is the same as that of Example 1 for the sealing agent resistant to high temperatures.
The crosslinking reaction may not occur at normal temperature for the sealing agent resistant to high temperatures, not plastic, and apparent viscosity at normal temperature is
119mPas stands 4 hours at 120 DEG C and cross-linking reaction takes place, and stands the gel strength that 8 hours form and reaches maximum, this
When colloid viscosity be 125463mPas, elasticity modulus 485Pa, viscous modulus 327Pa, 20 μm2It is held after reservoir core plugging
Pressure is 11.8MPa.The performance of the sealing agent can be stably kept 70 days at 120 DEG C.
Embodiment 9
The present embodiment provides a kind of sealing agent resistant to high temperatures, which is included the following components'mass percentage:
Polyacrylamide, 3%；
Sulfonated phenol formaldehyde resin, 1.2%；
Water swelling type particle sealing agent, 5%；
Hexa, 0.9%；
Uniaxial pressure sealer, 3%；
Sodium hydroxide, 3%；
Water, 83.9%.
The preparation method is the same as that of Example 1 for the sealing agent resistant to high temperatures.
The crosslinking reaction may not occur at normal temperature for the sealing agent resistant to high temperatures, not plastic, and apparent viscosity at normal temperature is
118mPas stands 4 hours at 100 DEG C and cross-linking reaction takes place, and stands the gel strength that 8 hours form and reaches maximum, this
When colloid viscosity be 90179mPas, elasticity modulus 473Pa, viscous modulus 213.7Pa, 10 μm2It is held after reservoir core plugging
Pressure is 8.8MPa.The performance of the sealing agent can be stably kept 70 days at 100 DEG C.
Embodiment 10
The present embodiment provides a kind of sealing agent resistant to high temperatures, which is included the following components'mass percentage:
Polyacrylamide, 3%；
Sulfonated phenol formaldehyde resin, 2%；
Water swelling type particle sealing agent, 5%；
Hexa, 1.2%；
Uniaxial pressure sealer, 3%；
Sodium hydroxide, 3%；
Water, 82.8%.
The preparation method is the same as that of Example 1 for the sealing agent resistant to high temperatures.
The crosslinking reaction may not occur at normal temperature for the sealing agent resistant to high temperatures, not plastic, and apparent viscosity at normal temperature is
115mPas stands 3 hours at 100 DEG C and cross-linking reaction takes place, and stands the gel strength that 8 hours form and reaches maximum, this
When colloid viscosity be 100179mPas, elasticity modulus 498Pa, viscous modulus 259Pa, 15 μm2It is held after reservoir core plugging
Pressure is 10.5MPa.The performance of the sealing agent can be stably kept 70 days at 100 DEG C.
The nature parameters of the sealing agent resistant to high temperatures of 1 Examples 1 to 10 of table
To sum up, the embodiment of the invention provides a kind of sealing agents with good high temperature resistant property.The sealing agent is being crosslinked
There is lower viscosity and good mobile performance before forming colloid, convenient for construction；The colloid formed after crosslinking has
Higher intensity, and stability is good.The sealing agent is blocked especially suitable for the stratum to 80~150 DEG C of severe leakages,
To guarantee going on smoothly for drilling well.
The above is merely for convenience of it will be understood by those skilled in the art that technical solution of the present invention, not to limit
The present invention.All within the spirits and principles of the present invention, any modification, equivalent replacement, improvement and so on should be included in this
Within the protection scope of invention.
Claims (8)
1. a kind of sealing agent resistant to high temperatures, which is characterized in that the sealing agent resistant to high temperatures includes the following components'mass percentage:
Polyacrylamide, 2%~3%；
Sulfonated phenol formaldehyde resin, 1%~2%；
Hexa, 0.9%~2%；
Water swelling type particle sealing agent, 3%~5%；
Uniaxial pressure sealer, 2%~6%；
Alkaline pH adjusting agent, 0~3%；
Water, surplus；
The partial size of the water swelling type particle sealing agent be 1.2 millimeters hereinafter, the water swelling type particle sealing agent it is swollen
Swollen multiple is 3 times or more；
The partial size of the uniaxial pressure sealer is 0.28 millimeter or less.
2. sealing agent resistant to high temperatures according to claim 1, which is characterized in that the alkaline pH adjusting agent is selected from hydroxide
At least one of sodium, potassium hydroxide and ammonium hydroxide.
3. sealing agent resistant to high temperatures according to claim 1, which is characterized in that the mass percent of the alkaline pH adjusting agent
It is 0.5%~2%.
4. sealing agent resistant to high temperatures according to claim 1, which is characterized in that the mass percent of the hexa
It is 1%~2%.
5. sealing agent resistant to high temperatures according to claim 1, which is characterized in that the quality percentage of the uniaxial pressure sealer
Than being 3%~5%.
6. sealing agent resistant to high temperatures according to claim 1, which is characterized in that the number-average molecular weight of the polyacrylamide is
3000000~5,000,000.
7. a kind of preparation method of sealing agent resistant to high temperatures described in claim 1, which is characterized in that the preparation method include with
Lower step:
Polyacrylamide is dissolved in the water to obtain polyacrylamide solution by step a；
Sulfonated phenol formaldehyde resin and hexa are added in the polyacrylamide solution by step b, are stirred to complete
Polymer solution is obtained after dissolution；
Alkaline pH adjusting agent, water swelling type particle sealing agent and uniaxial pressure sealer are added to the polymerization by step c
In object solution, stirring is to after being completely dissolved up to the sealing agent resistant to high temperatures.
8. a kind of application of sealing agent resistant to high temperatures described in claim 1, which is characterized in that convey the sealing agent resistant to high temperatures
To the stratum missed, and the sealing agent resistant to high temperatures is made to stand 6 hours on the stratum or more；The stratum temperature on the stratum
Degree is 80~150 DEG C.
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| CN108531159B (en) * | 2018-04-11 | 2021-01-01 | 东北石油大学 | High-temperature plugging agent system for heavy oil thermal recovery oil reservoir |
| CN108627446B (en) * | 2018-06-11 | 2020-10-09 | 重庆科技学院 | Method for testing plugging capability of plugging agent for fracturing |
| CN108864982A (en) * | 2018-08-01 | 2018-11-23 | 伍淼 | A kind of circulating line sealing agent and preparation method |
| CN112980407B (en) * | 2019-12-02 | 2023-05-30 | 中国石油化工股份有限公司 | Temperature-controllable gel plugging agent and preparation method and application thereof |
| CN110954451B (en) * | 2019-12-06 | 2023-02-03 | 中国石油天然气股份有限公司 | Application concentration and application particle size optimization method of flexible gel particle plugging agent |
| CN114626279A (en) * | 2020-12-14 | 2022-06-14 | 中国石油化工股份有限公司 | Method for optimizing grain size grading of rigid particle plugging agent in fracture |
| CN112980033A (en) * | 2021-02-26 | 2021-06-18 | 菲克光学科技(常州)有限公司 | Long-acting anti-static acrylic plate and preparation method thereof |
| CN113045719B (en) * | 2021-03-23 | 2022-11-08 | 中国石油大学(华东) | Plugging agent suitable for water plugging of high-temperature high-salinity clastic rock oil reservoir and preparation method thereof |
| CN115746808B (en) * | 2021-09-06 | 2024-04-30 | 中国石油天然气股份有限公司 | Plugging agent and application thereof |
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