CN109536144A - A kind of low temperature magnesium oxysulfide thermosetting resin gelling system and preparation method thereof - Google Patents
A kind of low temperature magnesium oxysulfide thermosetting resin gelling system and preparation method thereof Download PDFInfo
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- CN109536144A CN109536144A CN201710856214.2A CN201710856214A CN109536144A CN 109536144 A CN109536144 A CN 109536144A CN 201710856214 A CN201710856214 A CN 201710856214A CN 109536144 A CN109536144 A CN 109536144A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/42—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells
- C09K8/46—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells containing inorganic binders, e.g. Portland cement
- C09K8/467—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells containing inorganic binders, e.g. Portland cement containing additives for specific purposes
- C09K8/473—Density reducing additives, e.g. for obtaining foamed cement compositions
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/42—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells
- C09K8/46—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells containing inorganic binders, e.g. Portland cement
- C09K8/467—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells containing inorganic binders, e.g. Portland cement containing additives for specific purposes
- C09K8/48—Density increasing or weighting additives
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/42—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells
- C09K8/46—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells containing inorganic binders, e.g. Portland cement
- C09K8/467—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells containing inorganic binders, e.g. Portland cement containing additives for specific purposes
- C09K8/487—Fluid loss control additives; Additives for reducing or preventing circulation loss
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Abstract
The present invention relates to a kind of low temperature magnesium oxysulfide thermosetting resin gelling systems in oil gas well cementing operation field and preparation method thereof.The low temperature magnesium oxysulfide thermosetting resin gelling system slurry rheology is good, is easy to cementing operation.By using thermosetting resin cementitious material, consolidation bulk modulus can effectively reduce, increase consolidation body elasticity, improve impact resistance.It can further improve or regulate and control the performances such as density, rheology, curing time and the concretion body strength of aathermoset resin system with the use of magnesium oxysulfide framework material.Utilize the good bonding capacity of thermosetting resin, magnesium oxysulfide and metal, the expansion characteristics of magnesia improve the cementing strength at an interface and second interface, while meeting casing and cementing basic demand, the problems such as easily damaged, cementing difference existing for oil-well cement can also be solved, overcome the correlation of oil-well cement insufficient.Low temperature magnesium oxysulfide thermosetting resin gelling system of the invention is to have broad application prospects provides the art a kind of new selection.
Description
Technical field
The present invention relates to oil gas well cementing operation fields, furtherly, are related to a kind of low temperature magnesium oxysulfide thermosetting resin gel
System and preparation method thereof.
Background technique
Common oil-well cement is portland cement at present, and main chemical compositions are the oxides such as calcium oxide, silica, can
Cement slurry is mixed in a certain ratio into various extra materials, additive and water, and can be according to field demand to cement slurry density, solid
Change time etc. adjusts accordingly, and the Behavior of Hardened Cement Paste with certain compression strength, permeability resistance and durability is formed in underground.In view of
The good adaptability of portland cement has been widely used in all kinds of operations such as oil/gas well, complete well, well workover, has ensured oil gas field
Smooth exploitation.
However, as demand of the various countries to clean energy resource in recent years constantly increases, natural gas and unconventional petroleum resources
It is large-scale developed and utilized, but the work measures such as extensive acid fracturing make conventional silicate hardened oilwell cement expose height
The critical defects such as volume contraction, low elasticity.Its high volume contraction disadvantage makes cement sheath and borehole wall loop pipe bonding quality be deteriorated,
And microgap is formed in interface, lead to formation fluid channelling；Its low elasticity disadvantage makes cement sheath be subjected to the strong allergic effect of pit shaft
Masterpiece used time, easily-deformable destruction seriously affect cement sheath sealing performance, cause formation fluid channelling to well head, cause well head band
Pressure.Further, since often containing H in formation fluid2S、CO2Equal sour gas, with production operation carry out can gradually invade oil
Well annular space causes the corrosion of overbasic silicate cement mudstone, so as to cause the destruction of annular space leakproofness.Once cement sheath sealing is lost
Effect, remedial measure is less, costly, and it is lower to remedy success rate.General light, burnt masonry dam that middle petrochemical industry is gone into operation successively in recent years etc.
Different degrees of annular space problem with pressure is presented in gas field, wherein Behavior of Hardened Cement Paste deficiency itself be cause the problem major reason it
One.Therefore develop a kind of novel gelled material to solve the problems, such as current oil/gas well annular channeling, it appears it is particularly important with it is urgent,
It is the hot spot of recent domestic oil gas well cementing operation new material research and development.
Thermosetting resin refers to be chemically reacted under the effect of heating, pressurization or curing agent, and crosslinking curing generates insoluble
An insoluble resinoid, is cross-linked to form by intermolecular with three-dimensional grid structure, and intensity with higher.Common heat
Gu resin has phenolic resin, Lauxite, epoxy resin, melamine resin, polyurethane, furane resins etc..Have benefited from
The excellent mechanics of resin, thermodynamics, chemical stability, as coating, adhesive, moulding material etc. electronics, engineering technology,
The fields such as civil construction and stationery sports goods manufacture are widely applied, and direct and indirect use form almost spreads all works
Industry field, but in oil gas well cementing operation field using less.
The air hardening cementitious materials that magnesium oxysulfide cementitious material is formed by activated magnesia and Adlerika have quality
Gently, the excellent performances such as cohesive force is strong, impact resistance, thermal coefficient are low, and under stemness environment, compression strength and flexural strength
Increase with age, and sufficiently stable, therefore is widely used in building field.But there is also water-fast for magnesium oxysulfide cementitious material
Property poor, the limitation such as setting time is short and not easy to control, there is no research to apply in oil gas well cementing operation field.
Summary of the invention
In order to solve the problems, such as that above-mentioned portland cement performance existing in the prior art is insufficient, the present invention proposes a kind of low
Warm magnesium oxysulfide thermosetting resin gelling system.Relate in particular to a kind of low temperature magnesium oxysulfide thermosetting resin gelling system and its preparation side
Method.The low temperature magnesium oxysulfide thermosetting resin gelling system can realize that the part to existing cementing slurry is replaced under special circumstances
In generation, improves annular space sealing performance, realizes long-term to casing annulus efficiently cementing and sealing, reduces oil/gas well later period repairing work,
Reduce operation oil/gas well operating cost.The Sulfur-Vapor of Lower Temperature oxygen thermosetting resin gelling system rheological characteristic is good, and be easy to cement the well pump note construction.
One of the object of the invention is to provide a kind of low temperature magnesium oxysulfide thermosetting resin gelling system, may include that resin, resin are solid
The groups such as agent, magnesium oxysulfide framework material, low temperature adjustable solidification agent and fluid loss agent are grouped as；The magnesium oxysulfide framework material is by light-burned
Magnesia and magnesium sulfate composition.
Specifically, may include by the weight of light calcined magnesia be 100 parts by weight in terms of following components:
100 parts by weight of light calcined magnesia；
5~30 parts by weight of resin, preferably 10~25 parts by weight；
5~15 parts by weight of resin curing agent, preferably 7~15 parts by weight；
10~200 parts by weight of magnesium sulfate, preferably 30~70 parts by weight；
2~15 parts by weight of low temperature adjustable solidification agent, preferably 5~15 parts by weight；
1~3 parts by weight of fluid loss agent,
0.05~0.8 parts by weight of defoaming agent, preferably 0.1~0.5 parts by weight；
0~200 parts by weight of 0~100 parts by weight of density palliative or density heavy weight additive,
30~150 parts by weight of fresh water.
The resin is including but not limited to Lauxite, epoxy resin, acrylic resin, phenolic resin, polyester resin, ammonia
At least one of base resin, wherein it is preferred that phenolic resin.
The resin curing agent include but is not limited to the compounds such as inorganic acids, aliphatic amine, alicyclic polyamine class or
Its mixture.The low temperature adjustable solidification agent is the mixing of one or more of citric acid, acetic acid, phosphoric acid, acetic acid, malonic acid
Object.The fluid loss agent can be selected from least one of polyvinyl alcohol fluid loss agent, AMPS multiple copolymer analog fluid loss agent.
The defoaming agent is at least one of organic silicon defoaming agent, lipid defoaming agent.The density palliative is selected from floating bead, glass
At least one of microballon, flyash；The density heavy weight additive is selected from least one of barite, Iron Ore Powder, iron powder.
Low temperature magnesium oxysulfide thermosetting resin gelling system is a kind of novel gelling mixed liquor, utilizes molecule between thermosetting resin itself
Or curing agent catalysis carries out polycondensation reaction and forms intensity tridimensional network with higher, magnesium oxysulfide cementitious material is filled in tree
Among rouge frame and itself aquation is gelled to be formed with some strength and stability induration.By changing resin emulsion, sulphur oxygen
The density of the conveniently adjusted gelling system of the composition ratio such as magnesium cementitious material, additive and extra material, rheology, curing time and solid
Knot body intensity.While meeting casing and cementing basic demand, existing portland cement can be preferably solved in oil/gas well application
In brittleness it is big, easily damaged the deficiencies of, can partially substitute existing silicate oil-well cement, improve annular space sealing quality, improve water
Mud ring leakproofness.
The low temperature magnesium oxysulfide thermosetting resin gelling system of the invention thickening time between 20~45 DEG C is adjustable, and density exists
1.20~2.50g/cm3Between it is adjustable.The gelling system feature is: can cross-linked rubber under certain temperature and pressure condition
Thermal stability that is solidifying to form the induration with certain compression strength and excellent resilient properties, relying on high-molecular organic material excellent
And chemical stability, the excellent mechanical property of inorganic coagulation material and durability, improve well cementation annular space bonding quality, realizes well cementation
Annular space long term seal.
The second object of the present invention is to a kind of preparation method of low temperature magnesium oxysulfide thermosetting resin gelling system is provided, it can
The following steps are included: by the amount weigh light calcined magnesia, magnesium sulfate, resin, resin curing agent, defoaming agent, low temperature adjustable solidification agent,
Fluid loss agent, fresh water, density palliative or density heavy weight additive；Again by magnesium sulfate, resin, resin curing agent, defoaming agent, low temperature tune
Solidifying agent, fluid loss agent, mixing of fresh water it is uniform mixing liquid；Uniform light calcined magnesia, density will be finally puddled under stiring
The mixed powder of palliative or density heavy weight additive is added in mixing liquid, is stirred evenly and is obtained Sulfur-Vapor of Lower Temperature oxygen magnesium thermosetting resin
Gelling system.
The invention adopts the above technical scheme has the advantage that
It is put forward for the first time and utilizes magnesium oxysulfide thermosetting resin gelling system for low-temperature oil-gas well well cementation field, make full use of sulphur oxygen
The good air hardening characteristic of magnesium cement and stronger bonding capacity, and by thermosetting resin improvement magnesium oxysulfide concrete water repelling property with it is resistance to
Corrosive nature.For the gelling system between 20~45 DEG C, the thickening time is adjustable, and density is in 1.20~2.50g/cm3Between can
It adjusts.Gelling system, which can be crosslinked gelling under certain temperature and pressure condition and be formed, has certain compression strength and favorable elasticity
The induration of energy realizes effective sealing to stemness annular space.
Effect of the invention
1. the slurry rheology of low temperature magnesium oxysulfide thermosetting resin gelling system configuration is good, be easy to cement the well pump note construction.2. leading to
It crosses using thermosetting resin cementitious material, can effectively enhance induration water-resistance and corrosion resistance, while improving consolidation mechanics
Performance can effectively reduce consolidation bulk modulus, improves consolidation body elasticity, increases induration elastic deformability.3. passing through tune
It is adjustable to can control thermosetting resin curing time in 20~45 DEG C for whole resin curing agent dosage.4. being used cooperatively magnesium oxysulfide bone
Frame material can further improve or regulate and control density, rheology, curing time and the concretion body strength of thermosetting resin gelling system.⑤
It is adjustable in 20~45 DEG C of thickening times to can control magnesium oxysulfide thermosetting resin gelling system by addition low temperature adjustable solidification agent.6. passing through
Using the good bonding capacity of thermosetting resin, magnesium oxysulfide and metal and the expansion characteristics of magnesia, an interface and two boundaries are improved
The cementing strength in face.While meeting casing and cementing basic demand, additionally it is possible to solve easily damaged, cementing existing for oil-well cement
The problems such as difference overcome the correlation of oil-well cement insufficient.Low temperature magnesium oxysulfide thermosetting resin gelling system of the invention mentions for this field
A kind of new selection has been supplied, has been had broad application prospects.
Specific embodiment
Below with reference to embodiment, the present invention is further illustrated.But the present invention is not restricted by the embodiments.
Raw materials used in embodiment is commercially available.
Embodiment 1
(1) light calcined magnesia 300g, magnesium sulfate 150g are weighed, (Dezhou continental shelf is public by polyvinyl alcohol fluid loss agent FSAM-H
Department) 6g, low temperature adjustable solidification agent citric acid 20g, defoaming agent tributyl phosphate 1.5g, Phenolic resin emulsion (CNOOC Changzhou coating
Co., Ltd, work research institute) 60g, resin curing agent phosphoric acid 30g, fresh water 200g；
(2) magnesium sulfate, resin, resin curing agent, defoaming agent, low temperature adjustable solidification agent, fluid loss agent, mixing of fresh water is uniform
Mixing liquid；
(3) in the mixing container, mixing liquid is added, blender is rotated with (4000 ± 200 revs/min) of low speed, and 15
Light calcined magnesia powder is added in second, covers the lid of blender, and continue stirring 35 under high speed (12000 ± 500 revs/min)
Second, it stirs evenly and obtains Sulfur-Vapor of Lower Temperature oxygen magnesium thermosetting resin gelling system.According to the oil-well cement test side GB-T 19139-2012
Method measures density 1.65g/cm3, 20 DEG C of thickening time 320min, induration compression strength 18.6MPa, elasticity modulus 6.2GPa.
Embodiment 2
(1) light calcined magnesia 350g, magnesium sulfate 170g, polyvinyl alcohol fluid loss agent FSAM-H 6g, low temperature adjustable solidification agent are weighed
Citric acid 35g, defoaming agent tributyl phosphate 1.5g, Phenolic resin emulsion 50g, resin curing agent phosphoric acid 25g, Iron Ore Powder 400g,
Fresh water 250g；
(2) magnesium sulfate, resin, resin curing agent, defoaming agent, low temperature adjustable solidification agent, polyvinyl alcohol fluid loss agent, fresh water are mixed
Uniform mixing liquid is closed, for use；
(3) light calcined magnesia, Iron Ore Powder are puddled uniformly, for use；
(4) in the mixing container, mixing liquid is added, blender is rotated with (4000 ± 200 revs/min) of low speed, and 15
Light calcined magnesia and iron ore powder mixture are added in second, covers the lid of blender, and under high speed (12000 ± 500 revs/min)
Continue stirring 35 seconds, stirs evenly and obtain Sulfur-Vapor of Lower Temperature oxygen magnesium thermosetting resin gelling system, density 2.40g/cm3, 30 DEG C of thickening
Time 240min, concretion body strength 12.3MPa, elasticity modulus 5.2GPa.
Embodiment 3
(1) light calcined magnesia 200g, magnesium sulfate 100g, polyvinyl alcohol fluid loss agent FSAM-H 6g, low temperature adjustable solidification agent are weighed
Acetic acid 30g, defoaming agent tributyl phosphate 1.5g, Phenolic resin emulsion 60g, resin curing agent phosphoric acid 30g, floating bead 200g, fresh water
300g；
(2) magnesium sulfate, resin, resin curing agent, defoaming agent, low temperature adjustable solidification agent, fluid loss agent, mixing of fresh water is uniform
Mixing liquid, for use；
(3) light calcined magnesia, floating bead are puddled uniformly, for use；
(4) in the mixing container, mixing liquid is added, blender is rotated with (4000 ± 200 revs/min) of low speed, and 15
Add light calcined magnesia and floating bead mixture in second, cover the lid of blender, and under (6000 ± 500 revs/min) at a high speed after
Continuous stirring 35 seconds, stirs evenly and obtains Sulfur-Vapor of Lower Temperature oxygen magnesium thermosetting resin gelling system, density 1.25g/cm3, when 40 DEG C of thickening
Between 200min, concretion body strength 13.2MPa, elasticity modulus 5.6GPa.
Claims (9)
1. a kind of low temperature magnesium oxysulfide thermosetting resin gelling system, includes following components based on parts by weight:
100 parts by weight of light calcined magnesia；
5~30 parts by weight of resin, preferably 10~25 parts by weight；
5~15 parts by weight of resin curing agent, preferably 7~15 parts by weight；
10~200 parts by weight of magnesium sulfate, preferably 30~70 parts by weight；
2~15 parts by weight of low temperature adjustable solidification agent, preferably 5~15 parts by weight；
1~3 parts by weight of fluid loss agent；
0.05~0.8 parts by weight of defoaming agent, preferably 0.1~0.5 parts by weight；
0~200 parts by weight of 0~100 parts by weight of density palliative or density heavy weight additive；
30~150 parts by weight of fresh water.
2. a kind of low temperature magnesium oxysulfide thermosetting resin gelling system according to claim 1, it is characterised in that comprising with weight
The following components of number meter:
100 parts by weight of light calcined magnesia；
10~25 parts by weight of resin；
7~15 parts by weight of resin curing agent；
30~70 parts by weight of magnesium sulfate；
5~15 parts by weight of low temperature adjustable solidification agent；
1~3 parts by weight of fluid loss agent；
0.1~0.5 parts by weight of defoaming agent；
0~200 parts by weight of 0~100 parts by weight of density palliative or density heavy weight additive；
30~150 parts by weight of fresh water.
3. a kind of low temperature magnesium oxysulfide thermosetting resin gelling system according to claim 1 or 2, it is characterised in that:
The resin in Lauxite, epoxy resin, acrylic resin, phenolic resin, polyester resin, amino resins extremely
Few one kind, wherein it is preferred that phenolic resin.
4. a kind of low temperature magnesium oxysulfide thermosetting resin gelling system according to claim 1 or 2, it is characterised in that:
The resin curing agent is selected from least one of inorganic acids, aliphatic amine, alicyclic polyamine class.
5. a kind of low temperature magnesium oxysulfide thermosetting resin gelling system according to claim 1 or 2, it is characterised in that:
The low temperature adjustable solidification agent is selected from least one of citric acid, acetic acid, phosphoric acid, acetic acid, malonic acid.
6. a kind of low temperature magnesium oxysulfide thermosetting resin gelling system according to claim 1 or 2, it is characterised in that:
The fluid loss agent is selected from least one of polyvinyl alcohol fluid loss agent, AMPS multiple copolymer analog fluid loss agent.
7. a kind of low temperature magnesium oxysulfide thermosetting resin gelling system according to claim 1 or 2, it is characterised in that:
The defoaming agent is at least one of organic silicon defoaming agent, lipid defoaming agent.
8. a kind of low temperature magnesium oxysulfide thermosetting resin gelling system according to claim 1 or 2, it is characterised in that:
The density palliative is selected from least one of floating bead, glass microballoon, flyash；It is brilliant that the density heavy weight additive is selected from weight
At least one of stone, Iron Ore Powder, iron powder.
9. described in any item a kind of preparation methods of low temperature magnesium oxysulfide thermosetting resin gelling system according to claim 1~8,
The following steps are included: by the amount weigh light calcined magnesia, magnesium sulfate, resin, resin curing agent, defoaming agent, low temperature adjustable solidification agent,
Fluid loss agent, fresh water, density palliative or density heavy weight additive；Again by magnesium sulfate, resin, resin curing agent, defoaming agent, low temperature tune
Solidifying agent, fluid loss agent, mixing of fresh water it is uniform mixing liquid；Uniform light calcined magnesia, density will be finally puddled under stiring
The mixed powder of palliative or density heavy weight additive is added in mixing liquid, is stirred evenly and is obtained Sulfur-Vapor of Lower Temperature oxygen magnesium thermosetting resin
Gelling system.
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| CN111460678A (en) * | 2020-04-16 | 2020-07-28 | 四川大学 | Filling rate optimization method of cement cementing material |
| CN114196387A (en) * | 2021-07-16 | 2022-03-18 | 中国石油天然气集团有限公司 | Shear-dilution type acid-soluble inorganic curing plugging agent, and preparation method and application thereof |
| CN115677317A (en) * | 2022-10-24 | 2023-02-03 | 千年舟新材科技集团股份有限公司 | Multi-component class-A fireproof facing layer material, class-A fireproof plate and preparation method of class-A fireproof facing layer material |
| CN117025188A (en) * | 2023-10-10 | 2023-11-10 | 中国石油大学(华东) | Low-thermal-conductivity additive for deep water shallow layer well cementation as well as preparation method and application thereof |
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| CN117025188A (en) * | 2023-10-10 | 2023-11-10 | 中国石油大学(华东) | Low-thermal-conductivity additive for deep water shallow layer well cementation as well as preparation method and application thereof |
| CN117025188B (en) * | 2023-10-10 | 2024-01-12 | 中国石油大学(华东) | Low-thermal-conductivity additive for deep water shallow layer well cementation as well as preparation method and application thereof |
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