CN106336477A - Capsule-coat-thickness adjustable microcapsule gel breaking agent and preparation method thereof - Google Patents
Capsule-coat-thickness adjustable microcapsule gel breaking agent and preparation method thereof Download PDFInfo
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- CN106336477A CN106336477A CN201610705386.5A CN201610705386A CN106336477A CN 106336477 A CN106336477 A CN 106336477A CN 201610705386 A CN201610705386 A CN 201610705386A CN 106336477 A CN106336477 A CN 106336477A
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- China
- Prior art keywords
- capsule
- thickness adjustable
- coat
- degelling agent
- ammonium persulfate
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/04—Acids; Metal salts or ammonium salts thereof
- C08F220/06—Acrylic acid; Methacrylic acid; Metal salts or ammonium salts thereof
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/06—Making microcapsules or microballoons by phase separation
- B01J13/14—Polymerisation; cross-linking
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/44—Polymerisation in the presence of compounding ingredients, e.g. plasticisers, dyestuffs, fillers
-
- 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
- C09K8/60—Compositions for stimulating production by acting on the underground formation
- C09K8/62—Compositions for forming crevices or fractures
- C09K8/66—Compositions based on water or polar solvents
- C09K8/68—Compositions based on water or polar solvents containing organic compounds
-
- 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
- C09K8/60—Compositions for stimulating production by acting on the underground formation
- C09K8/62—Compositions for forming crevices or fractures
- C09K8/70—Compositions for forming crevices or fractures characterised by their form or by the form of their components, e.g. foams
- C09K8/706—Encapsulated breakers
-
- 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
- C09K8/60—Compositions for stimulating production by acting on the underground formation
- C09K8/84—Compositions based on water or polar solvents
- C09K8/86—Compositions based on water or polar solvents containing organic compounds
- C09K8/88—Compositions based on water or polar solvents containing organic compounds macromolecular compounds
- C09K8/882—Compositions based on water or polar solvents containing organic compounds macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K2208/00—Aspects relating to compositions of drilling or well treatment fluids
- C09K2208/26—Gel breakers other than bacteria or enzymes
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Dispersion Chemistry (AREA)
- Manufacturing Of Micro-Capsules (AREA)
Abstract
The invention discloses a capsule-coat-thickness adjustable microcapsule gel breaking agent and a preparation method thereof, the capsule-coat-thickness adjustable microcapsule gel breaking agent comprises the following components by weight: 16-17 parts of ammonium persulfate or potassium persulfate, 19-24 parts of polymerization monomers and 0.06-0.07 part of an initiator; the polymerization monomers include methacrylic acid, methyl methacrylate, ethyl methacrylate and styrene which are fed in a certain proportion, the capsule-coat-thickness adjustable microcapsule gel breaking agent takes the ammonium persulfate or the potassium persulfate as a capsule core, capsule coats with different thickness are prepared from the four polymerization monomers of methacrylic acid, methyl methacrylate, ethyl methacrylate and styrene through polymerization by in-situ polymerization method, by effective control of time for the ammonium persulfate or the potassium persulfate entering a solution by diffusion, gel breaking time is effectively delayed to a time range of 130-200min, at the same time, after a hydroxypropyl guanidine gum fracturing fluid is added into the capsule-coat-thickness adjustable microcapsule gel breaking agent, under atmospheric pressure at 90 DEG C, after shearing for 50min in 170s<-1>, viscosity is still greater than 200mPa.S, and suspending sand requirements can be met.
Description
Technical field
The present invention relates to technical field of petroleum extraction, particularly to a kind of peel thickness adjustable type microcapsule degelling agent and its
Preparation method.
Background technology
Horizontal well multistage subsection fracturing technique is more and more extensive in the application of national each oil gas field.This technical requirements is all each
Fracturing fluid in section unified broken glue after construction terminates returns discharge ground.The fracturing fluid time of staying in early stage fracturing section is longer,
Change water to spread in stratum in the presence of gel breaker, the secondary pollution on stratum prolongation over time is increased.This just needs
To regulate and control the broken glue time of fracturing fluid by adding the method for capsule breaker.
At present mining site construction usage mainly with Ammonium persulfate. as capsule-core, the capsule breaker as peel for the paraffin.Such
The releasing mechanism of type gel breaker is mainly film rupture, i.e. peel rupture under the collective effect of strata pressure and temperature, discharges
Ammonium persulfate. produces broken glue effect.From the point of view of the preparation method and the broken glue effect of laboratory of the type capsule breaker, peel
Optional species is less, the regulation of peel thickness is uncontrollable, thus can not reach the effect of manual control on the broken glue time.
In recent years the research of capsule breaker is expanded to using polymer as peel, gathered by choosing adaptability monomer
Close and obtain different peels, thus controlling water to enter glue microcapsule degelling agent realize broken glue;Its concrete rubber breaker reason is hydrone
Capsule-core dissolving gel breaker is entered by the polymeric membrane after swelling, the gel breaker after dissolving goes out capsule by concentration difference diffusion flow
Outward, thus playing brokenly glue effect.The feature of this class gel breaker is to control by changing peel structure and peel thickness
The peel processed swelling time, and then control Ammonium persulfate. class oxidant to diffuse into the time of solution, reach brokenly the glue time controlled
Purpose.
Content of the invention
It is an object of the invention to provide one kind can be realized controlling water to enter in capsule by adjusting ratio between polymerized monomer
The peel thickness adjustable type microcapsule degelling agent of portion's time.
It is a further object of the present invention to provide one kind prepares above-mentioned peel thickness adjustable type microcapsule using situ aggregation method
The preparation method of gel breaker.
For this reason, technical solution of the present invention is as follows:
A kind of peel thickness adjustable type microcapsule degelling agent, including following components in parts by weight:
Ammonium persulfate. or potassium peroxydisulfate 16~17 weight portion,
Polymerized monomer 19~24 weight portion,
Initiator 0.06~0.07 weight portion,
Wherein, described polymerized monomer includes methacrylic acid, methyl methacrylate, ethyl methacrylate and benzene second
Alkene;Preferably, four kinds of polymerized monomer methacrylic acids, methyl methacrylate, ethyl methacrylate and cinnamic material
The ratio of amount is (0.9~1.3): (0.45~0.55): (0.2~0.35): (0.25~0.35).
Preferably, described initiator is azo-bis-iso-dimethyl or azo two isobutyl imidazoline hydrochloride.
A kind of preparation method of peel thickness adjustable type microcapsule degelling agent, concretely comprises the following steps: by Ammonium persulfate. or over cure
Sour potassium is dissolved in water the saturated solution being configured to Ammonium persulfate. or potassium peroxydisulfate, and the ph value adjusting solution, to 1~3, adds poly-
Close the alcoholic solution of monomer and stir to being completely dissolved rear heating in water bath to 68~72 DEG C;Will be slow for the described mixed solution after heating
Instill in chloroform, instill the alcoholic solution being dissolved with initiator, 68~72 DEG C of stirring 4.5~5.5h of constant temperature simultaneously;To obtain
Product filter and with absolute ethanol washing repeatedly, be dried, you can obtain microcapsule degelling agent.
Preferably, described ph regulator is hydrochloric acid.
Preferably, a kind of preparation method of peel thickness adjustable type microcapsule degelling agent, concretely comprises the following steps:
(1) preparation in a certain amount of water will be dissolved under the Ammonium persulfate. of 16~17 weight portions or potassium peroxydisulfate normal temperature condition
Become Ammonium persulfate. saturated solution, the ph value adjusting solution is to 1~3;
(2) the four kinds of polymerizations through ethanol dissolving sequentially adding 19~24 weight portions in the solution being obtained to step (1) are single
The alcoholic solution of body mixture, four kinds of polymer monomer methacrylic acids, methyl methacrylate, ethyl methacrylate and benzene second
The ratio of the amount of the material of alkene is (0.9~1.3): (0.45~0.55): (0.2~0.35): (0.25~0.35), stirs to complete
After dissolving, heating in water bath is to 68~72 DEG C;
(3) mixed solution that step (2) is obtained is slowly dropped into while hot and fills three mouthfuls of 14~25 weight portion chloroform
In bottle, instill the solution being dissolved with 0.06~0.07 weight portion initiator, 68~72 DEG C of stirring 4.5~5.5h of constant temperature simultaneously, obtain
To solidliquid mixture;
(4) will filter through the product that step (3) obtain and with absolute ethanol washing repeatedly, be dried, you can obtain microcapsule
Gel breaker.
During fracturing work, addition in fracturing fluid for this microcapsule degelling agent is 0.01~0.05wt%.
Compared with prior art, this peel thickness adjustable type microcapsule degelling agent is with Ammonium persulfate. or potassium peroxydisulfate as capsule
Core, methacrylic acid, methyl methacrylate, ethyl methacrylate and four kinds of polymerized monomers of styrene pass through situ aggregation method
Polymerization is formed has the peel of different-thickness, and effective control Ammonium persulfate. or potassium peroxydisulfate diffuse into the time of solution, realize
Delay timing breaks the effect of glue;Using the microcapsule degelling agent of said method preparation make brokenly the glue time be effectively delayed to 130~
In the time range of 200min, after it is added into hydroxypropyl guar fracturing fluid, under the conditions of 90 DEG C of normal pressure, in 170s simultaneously-1, shearing
After 50min, viscosity, still above 200mpa s, disclosure satisfy that outstanding sand requirement.
Brief description
Fig. 1 is that the peel thickness adjustable type microcapsule degelling agent of the embodiment of the present invention 1 preparation is cut under the conditions of 90 DEG C of normal pressure
Cut viscosity to scheme over time;
The peel thickness adjustable type microcapsule degelling agent of Fig. 2 embodiment of the present invention 2 preparation is in 90 DEG C of condition down cuts of normal pressure
Viscosity is schemed over time;
The peel thickness adjustable type microcapsule degelling agent of Fig. 3 embodiment of the present invention 3 preparation is in 90 DEG C of condition down cuts of normal pressure
Viscosity is schemed over time.
Specific embodiment
Below in conjunction with the accompanying drawings and specific embodiment the present invention is described further, but following embodiment is absolutely not to this
Bright have any restriction.
Embodiment 1
16.1g Ammonium persulfate. is dissolved in 20.64g water and is configured to Ammonium persulfate. saturated solution, and adjusted with hydrochloric acid molten
The ph value of liquid, to 2, then sequentially adds 8.23g methacrylic acid, 4.85g methyl methacrylate, 2.67g methyl in solution
Ethyl acrylate and 3.6g styrene are dissolved in the alcoholic solution formed in dehydrated alcohol and stir to being completely dissolved rear heating in water bath
To 70 DEG C;Mixed solution after heating is slowly dropped in 24.49g chloroform while hot, instills simultaneously and be dissolved with 0.07g azo
The ethanol solution of two isobutyl dimethyl phthalates, 70 DEG C of stirring 5h of constant temperature;The product obtaining is filtered and multiple with absolute ethanol washing,
It is dried, you can obtain microcapsule degelling agent i.
It is illustrated in figure 1 concentration 0.03% by mass percentage and microcapsule degelling agent i is added into hydroxypropyl guar pressure break
Liquid rear overhang sand changes over the viscosity B coefficent curve of fracturing fluid.
From figure 1 it appears that under the conditions of 90 DEG C of normal pressure, 170s-1, shearing 50min after viscosity be more than 200mpa s,
Meet outstanding sand to require;After 170min, the viscosity of fracturing fluid is reduced to 50mpa s, and after 200min, viscosity < 10mpa s, reaches brokenly
Glue returns the standard of discharge opeing.
It can be seen that, the broken glue time of the microcapsule degelling agent i of embodiment 1 preparation is 200min.
Embodiment 2
16.34g Ammonium persulfate. is dissolved in 20.92g water and is configured to Ammonium persulfate. saturated solution, and adjusted with hydrochloric acid molten
The ph value of liquid, to 2, then sequentially adds 11.62g methacrylic acid, 5.17g methyl methacrylate, 3.83g first in solution
Base ethyl acrylate and 3.28g styrene are dissolved in the alcoholic solution formed in dehydrated alcohol stirring to being completely dissolved rear water-bath and add
Heat is to 70 DEG C;Mixed solution after heating is slowly dropped in 14.88g chloroform while hot, instills simultaneously and be dissolved with 0.06g occasionally
The ethanol solution of nitrogen two isobutyl dimethyl phthalate, 70 DEG C of stirring 5h of constant temperature;The product obtaining is filtered and many with absolute ethanol washing
Secondary, it is dried, you can obtain microcapsule degelling agent ii.
It is illustrated in figure 2 concentration 0.03% by mass percentage and microcapsule degelling agent ii is added into hydroxypropyl guar pressure break
Liquid rear overhang sand changes over the viscosity B coefficent curve of fracturing fluid.
From figure 2 it can be seen that under the conditions of 90 DEG C of normal pressure, 170s-1, shearing 50min after viscosity be more than 200mpa s,
Meet outstanding sand to require;After 140min, the viscosity of fracturing fluid is reduced to 50mpa s, and after 170min, viscosity < 10mpa s, reaches brokenly
Glue returns the standard of discharge opeing.
It can be seen that, the broken glue time of the microcapsule degelling agent ii of embodiment 2 preparation is 170min.
Embodiment 3
16.18g Ammonium persulfate. is dissolved in 20.53g water and is configured to Ammonium persulfate. saturated solution, and adjusted with hydrochloric acid molten
The ph value of liquid, to 2, then sequentially adds 10.83g methacrylic acid, 4.63g methyl methacrylate, 3.18g first in solution
Base ethyl acrylate and 2.99g styrene are dissolved in the alcoholic solution formed in dehydrated alcohol stirring to being completely dissolved rear water-bath and add
Heat is to 70 DEG C;Mixed solution after heating is slowly dropped in 19.96g chloroform while hot, instills simultaneously and be dissolved with 0.06g occasionally
The ethanol solution of nitrogen two isobutyl dimethyl phthalate, 70 DEG C of stirring 5h of constant temperature;The product obtaining is filtered and many with absolute ethanol washing
Secondary, it is dried, you can obtain microcapsule degelling agent iii.
It is illustrated in figure 3 concentration 0.03% by mass percentage and microcapsule degelling agent iii is added into hydroxypropyl guar pressure
Split the viscosity B coefficent curve that liquid rear overhang sand changes over fracturing fluid.
From figure 3, it can be seen that under the conditions of 90 DEG C of normal pressure, 170s-1, shearing 50min after viscosity be more than 200mpa s,
Meet outstanding sand to require;After 110min, the viscosity of fracturing fluid is reduced to 50mpa s, and after 130min, viscosity < 10mpa s, reaches brokenly
Glue returns the standard of discharge opeing.
It can be seen that, the broken glue time of the microcapsule degelling agent iii of embodiment 3 preparation is 130min.
In sum, to cross Ammonium persulfate. or potassium peroxydisulfate as capsule-core, cooperation methacrylic acid, methyl methacrylate,
Four kinds of polymerized monomer in-situ polymerizations of ethyl methacrylate and styrene are the microcapsule degelling agent energy that the different peel of thickness is formed
Enough effective delay timings break the effect of glue.
Claims (5)
1. a kind of peel thickness adjustable type microcapsule degelling agent is it is characterised in that include following components in parts by weight: 16~17 parts
Ammonium persulfate. or potassium peroxydisulfate, 19~24 parts of polymerized monomers and 0.06~0.07 part of initiator;Wherein, described polymerized monomer includes
Methacrylic acid, methyl methacrylate, ethyl methacrylate and styrene.
2. peel thickness adjustable type microcapsule degelling agent according to claim 1 is it is characterised in that in four kinds of polymerized monomers
Methacrylic acid, the ratio of the amount of methyl methacrylate, ethyl methacrylate and cinnamic material are (0.9~1.3):
(0.45~0.55): (0.2~0.35): (0.25~0.35).
3. peel thickness adjustable type microcapsule degelling agent according to claim 1 is it is characterised in that described initiator is even
Nitrogen two isobutyl dimethyl phthalate or azo two isobutyl imidazoline hydrochloride.
4. a kind of preparation method of peel thickness adjustable type microcapsule degelling agent is it is characterised in that concretely comprise the following steps: by persulfuric acid
Ammonium or potassium peroxydisulfate are dissolved in water the saturated solution being configured to Ammonium persulfate. or potassium peroxydisulfate, adjust the ph value of solution to 1~
3, add the alcoholic solution of polymerized monomer and stir to being completely dissolved rear heating in water bath to 68~72 DEG C;By the described mixing after heating
Solution is slowly dropped in chloroform, instills simultaneously and is dissolved with the alcoholic solution of initiator, and 68~72 DEG C of stirrings of constant temperature 4.5~
5.5h;The product obtaining is filtered and with absolute ethanol washing repeatedly, is dried, you can obtain microcapsule degelling agent.
5. the preparation method of peel thickness adjustable type microcapsule degelling agent according to claim 4 is it is characterised in that described
Ph regulator is hydrochloric acid.
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Cited By (4)
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CN108570313A (en) * | 2018-04-09 | 2018-09-25 | 西南石油大学 | A kind of oil well cement high temperature retarder microcapsules and preparation method thereof |
CN109203164A (en) * | 2018-09-20 | 2019-01-15 | 佛山市蓝瑞欧特信息服务有限公司 | It is a kind of to can be realized the floor repeatedly conserved and maintenance process |
CN112852401A (en) * | 2021-01-15 | 2021-05-28 | 常熟理工学院 | High-suspension dispersion type capsule gel breaker and preparation method thereof |
CN118165181A (en) * | 2024-05-13 | 2024-06-11 | 西南石油大学 | Preparation method and application of microcapsule delayed initiation gel system |
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Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108570313A (en) * | 2018-04-09 | 2018-09-25 | 西南石油大学 | A kind of oil well cement high temperature retarder microcapsules and preparation method thereof |
CN108570313B (en) * | 2018-04-09 | 2020-11-03 | 西南石油大学 | Oil well cement high-temperature retarder microcapsule and preparation method thereof |
CN109203164A (en) * | 2018-09-20 | 2019-01-15 | 佛山市蓝瑞欧特信息服务有限公司 | It is a kind of to can be realized the floor repeatedly conserved and maintenance process |
CN112852401A (en) * | 2021-01-15 | 2021-05-28 | 常熟理工学院 | High-suspension dispersion type capsule gel breaker and preparation method thereof |
CN112852401B (en) * | 2021-01-15 | 2022-03-29 | 常熟理工学院 | High-suspension dispersion type capsule gel breaker and preparation method thereof |
CN118165181A (en) * | 2024-05-13 | 2024-06-11 | 西南石油大学 | Preparation method and application of microcapsule delayed initiation gel system |
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Application publication date: 20170118 |