CN109749726A - A kind of medium temperature phosphate thermosetting resin gelling system and preparation method thereof - Google Patents
A kind of medium temperature phosphate thermosetting resin gelling system and preparation method thereof Download PDFInfo
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- CN109749726A CN109749726A CN201711063750.3A CN201711063750A CN109749726A CN 109749726 A CN109749726 A CN 109749726A CN 201711063750 A CN201711063750 A CN 201711063750A CN 109749726 A CN109749726 A CN 109749726A
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- thermosetting resin
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- temperature phosphate
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Abstract
The present invention relates to a kind of medium temperature phosphate thermosetting resin gelling systems in oil gas well cementing operation field and preparation method thereof.The medium temperature phosphate thermosetting resin gelling system, thermosetting resin, the phosphate cement contained in system can be formed by curing with advantages of higher compressive strength under wellbore environment, compared with low elastic modulus, compared with the Behavior of Hardened Cement Paste of low-permeability, and Behavior of Hardened Cement Paste anticorrosion effect is good, can effectively increase sealing validity period of the cement sheath in acid medium.By using auxiliary resin curing agent, retarder, which can use within the temperature range of 45~80 DEG C, and integrally the pumpable time meets site operation requirement to system.Medium temperature phosphate thermosetting resin gelling system can be realized under the hole condition of part to all or part substitution of silicate oil-well cement, more effectively realize the complete seal of pit shaft, provide a kind of novel working solution system for oil gas well cementing operation, with good application prospect.
Description
Technical field
The present invention relates to oil gas well cementing operation field working solutions, furtherly, are related to a kind of medium temperature phosphate thermosetting tree
Rouge gelling system and preparation method thereof.
Background technique
Currently, silicate oil-well cement is the common cementitious material of oil gas well cementing operation, main component is calcium silicates substrate
Material may occur from body hydration reaction after meeting water, and can under certain temperature, pressure condition harden(ing)by itself at solid cement
Stone.Have benefited from the hydraulically active of its silicate material, silicate oil-well cement and various aqueous admixtures (fluid loss agent, slow setting
Agent etc.) excellent fit 5, the slurry with certain fluidity is formed, and can realize by blending various inorganic material to slurry
Mitigation or exacerbation.Because of the higher compression strength of silicate cement mudstone itself, lower permeability, preferable durability, substantially
Meet oil/gas well job requirements, therefore applies very universal in the operations such as conventional oil gas well cementing, complete well.But silicate cement
Mudstone also has the defect of itself, one is the hard brittleness under advantages of higher compressive strength, so that Behavior of Hardened Cement Paste is by biggish outer masterpiece
Used time itself destroys；The second is autogenous shrinkage, silicate material is in itself hydration process, due to hydrated product crystal form
Transformation so that Behavior of Hardened Cement Paste overall volume reduce.Defect results in pit shaft cement sheath and is easily broken thereon, cement sheath and casing, water
Mud ring and the borehole wall form microannulus, to seriously affect effective packing to annular space of Behavior of Hardened Cement Paste, cause formation fluid alter to
Well head influences production safety.Therefore, improving the hard brittleness of silicate cement mudstone itself, making up autogenous shrinkage is oil/gas well in recent years
The pressing issues that well cementation faces.
Summary of the invention
In order to solve the above-mentioned problems in the prior art, the present invention proposes a kind of medium temperature phosphate thermosetting resin gelling
System.Relate in particular to a kind of medium temperature phosphate thermosetting resin gelling system and preparation method thereof.The medium temperature phosphate heat
Gu resin gelling system itself can be gelled under temperature in wellbore, pressure, be frozen into higher resistance to compression after injecting pit shaft
The induration of intensity and durability, so that effective fixed sleeving, completely cuts off on fluid and alter, meet oil gas well cementing operation safe construction and ring
Empty seal request.The medium temperature phosphate thermosetting resin gelling system in 45~80 DEG C, by flow regime be gelled to it is solid when
Between can adjust according to demand, guarantee scene injection construction safety, can partially or completely substitute currently used silicate grout
System.
One of the object of the invention is to provide a kind of medium temperature phosphate thermosetting resin gelling system.The medium temperature phosphate thermosetting
Resin gelling system, the following components comprising parts by weight meter:
Wherein,
The thermosetting resin can be selected from one or more of melamine resin, furane resins, epoxy resin etc..
The resin curing agent can be selected from the resin solidification of aliphatic category, aliphatic amine, esters, sulfonic acid and Sulfonates
One or more of agent.
The phosphate can be selected from phosphoric acid, potassium dihydrogen phosphate, sodium dihydrogen phosphate, ammonium dihydrogen phosphate, in Quadrafos extremely
Few one or more.Phosphate cement itself aquation is condensed into advantages of higher compressive strength Behavior of Hardened Cement Paste, low alkalinity feature
It can make phosphate cement stone that there is excellent acid-alkali-corrosive-resisting performance；For thermosetting resin under resin curing agent effect, formation is insoluble not
Molten three-dimensional structure, and it is mutually interspersed with phosphate cement stone, and the mechanical property and corrosion resistance of collaboration enhancing induration increase
Add wall surface cementing strength, to realize the more permanent effectively sealing of annular space.
The metal oxide can be selected from dead burned magnesia, aluminium oxide, calcium oxide or other metal oxides at least
It is a kind of.Both the metal oxide and phosphate can be gelled to form phosphate cement stone.
The retarder can be selected from least one of citrate, boric acid, borax, can be inorganic salts, be also possible to
Organic salt etc..The retarder may make that the thickening time of medium temperature phosphate thermosetting resin gelling system is adjustable controllable.
The fluid loss agent can be in polyvinyl alcohol, cellulose family, lignin fluid loss agent
It is at least one.The fluid loss agent can reduce dehydration of the gelling system in pit shaft in flow process.
Mitigation therein or weighting material can be inorganic material, can also be organic material, specific optional glass freely
At least one of microballon, silicon powder, Iron Ore Powder, modified pitch etc..The gelling system can be mitigated by blending or weighting material is real
Existing density adjustment, meets the requirement under different well's conditions to slurry density, and slurry sedimentation stability is good.The application's is suitable for 45
~80 DEG C of medium temperature phosphate thermosetting resin gelling system density can by puddle mitigation or weighting material 1.20~
2.50g/cm3Between it is adjustable, the curing time of system can adjust between 30~300min by adjusting the dosage of retarder.
Resin in the gelling system can self-crosslinking consolidate to form three-dimensional net rack framework, phosphate cement also it is curable at
Phosphate cement stone, phosphate concrete is filled among resinous framework, phosphoric acid jelling structure and the three-dimensional netted knot of resin
The mutually interspersed effective packing for forming the induration with some strength and stability, realizing to annular space of structure, and keep for a long time close
Seal validity.By changing the conveniently adjusted glue of composition ratio such as resin emulsion, phosphate concrete, additive and extra material
Density, rheology, curing time and the concretion body strength of solidifying system.While meeting cementing slurry basic demand, induration
Excellent mechanical property can preferably solve the deficiencies of existing silicate cement mudstone brittleness is big, easily damaged, perishable caused water
Mud ring seal is every Problem of Failure.Existing portland cement can be partially substituted, annular space sealing quality can be improved, improves cement sheath sealing
Property.
The second object of the present invention is to providing the preparation method of the medium temperature phosphate thermosetting resin gelling system, it may include
Following steps:
Each component is weighed up by the dosage first spare；Secondly metal oxide, lightening material or weighting material is equal
It is even to puddle to obtain mixed powder；Again by phosphate, thermosetting resin, resin curing agent, retarder, fluid loss agent, mixing of fresh water
It is uniform to obtain mixing liquid；Finally mixed powder is added in mixing liquid under stiring, stirs evenly and obtains the medium temperature
Phosphate thermosetting resin gelling system.
Effect of the invention
1. the fluid ability that medium temperature phosphate thermosetting resin gelling system can be maintained for a long time at normal temperature, system thickening
Time is adjustable controllable in 45~80 DEG C of temperature ranges.2. gelling system can by the way that mitigation or weighting material, system density is added
In 1.20~2.50g/cm3Between it is adjustable, and slurry sedimentation stability is good.3. the thermoset material in gelling system is solid
The lower consolidation of agent effect, induration compression strength with higher, lower elasticity modulus, and consolidation time is in 45~80 DEG C of temperature
It spends adjustable controllable in range.4. the phosphate in gelling system has good with the phosphate cement stone that reactive metal oxide generates
Good compression strength, excellent acid resistance, gas attack performance and high temperature resistance.And by adjusting mating retarder dosage,
Phosphate cement firm time is adjustable controllable in 45~80 DEG C of temperature ranges.5. passing through both phosphate cement and thermosetting resin
Structure interpenetrating, collaboration enhancing concretion body strength and density and the durability in acid medium, effectively completely cut off wellbore fluids
Annular space long-term seal is realized in migration.The present invention has to prevent the migration of oil/gas well annular fluid from providing a kind of new gelling system
There is preferable application prospect.
Application field and application prospect of the invention
The present invention relates to a kind of well cementation medium temperature phosphate thermosetting resin gelling systems, are mainly used for medium temperature oil gas well cementing operation
Field makes up the deficiency of silicate Performances of Oil Well Cement under special circumstances, solves part well cementation problem.The medium temperature phosphate heat
Gu resin gelling system rheological characteristic is good, slurry be easy to cement the well pump note construction, it can be achieved that medium temperature condition lower curing time it is controllable, meet
Cementing operation condition.
The medium temperature phosphate thermosetting resin gelling system has stronger wall surface cementing power, and induration has good bullet
Property deformability, excellent impact resistance and corrosion resistance.The medium temperature phosphate thermosetting resin gelling system can be special
The slurry application of part substituted for silicon acid salt cement is realized under hole condition, is improved the leakproofness of annular space, is guaranteed the efficient production of oil/gas well, have
Preferable promotion and application value.
Specific embodiment
Below with reference to embodiment, the present invention is further illustrated.But the present invention is not restricted by the embodiments.
Embodiment 1
(1) 400g dead burned magnesia, potassium dihydrogen phosphate 100g, FSAM-H polyvinyl alcohol fluid loss agent 10g are weighed, medium temperature is delayed
Solidifying agent boric acid 10g, epoxy resin latex 60g, resin curing agent tetraethylenepentamine 30g, fresh water 200g.
(2) by potassium dihydrogen phosphate, thermosetting resin, resin curing agent, medium temperature retarder, polyvinyl alcohol fluid loss agent, fresh water
It is uniformly mixed to obtain 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 medium temperature phosphate thermosetting resin gelling system, density 1.60g/cm3, according to GB-T 19139-2012
Oil-well cement test method measures 45 DEG C of thickening time 380min, induration compression strength 20.2MPa/48h, elasticity modulus
7.6GPa。
Embodiment 2
(1) 300g dead burned magnesia, sodium dihydrogen phosphate 100g, FSAM-H polyvinyl alcohol fluid loss agent 16g are weighed, medium temperature is delayed
Solidifying agent boric acid 15g, epoxy resin latex 80g, resin curing agent tetraethylenepentamine 20g, fresh water 250g, glass microballoon 300g.
(2) dead burned magnesia, glass microballoon are puddled uniformly, for use；
(3) by sodium dihydrogen phosphate, thermosetting resin, resin curing agent, medium temperature retarder, polyvinyl alcohol fluid loss agent, fresh water
It is uniformly mixed to obtain mixing liquid, for use；
(4) in the mixing container, mixing liquid is added, blender is rotated with (4000 ± 200 revs/min) of low speed, and 15
Dead burned magnesia and glass microballoon mixture are added in second, covers the lid of blender, and in high speed (6000 ± 500 revs/min)
Under continue stirring 35 seconds, stir evenly and obtain medium temperature phosphate thermosetting resin gelling system, density 1.30g/cm3, 60 DEG C thick
Change time 290min, induration compression strength 18.2MPa/48h, elasticity modulus 6.9GPa.
Embodiment 3
(1) 250g dead burned magnesia, sodium dihydrogen phosphate 100g, FSAM-H polyvinyl alcohol fluid loss agent 20g are weighed, medium temperature is delayed
Solidifying agent boric acid 20g, epoxy resin latex 60g, resin curing agent tetraethylenepentamine 10g, fresh water 250g, Iron Ore Powder 300g.
(2) dead burned magnesia, Iron Ore Powder are puddled uniformly, obtains mixed powder, for use；
(3) by sodium dihydrogen phosphate, thermosetting resin, resin curing agent, medium temperature retarder, polyvinyl alcohol fluid loss agent, fresh water
It is uniformly mixed to obtain mixing liquid, for use；
(4) in the mixing container, mixing liquid is added, blender is rotated with (4000 ± 200 revs/min) of low speed, and 15
Dead burned magnesia and iron ore powder mixture are added in second, covers the lid of blender, and under high speed (6000 ± 500 revs/min)
Continue stirring 35 seconds, stirs evenly and obtain medium temperature phosphate thermosetting resin gelling system, density 2.30g/cm3, 80 DEG C of thickening
Time 220min, induration compression strength 15.3MPa/48h, elasticity modulus 6.2GPa.
Claims (10)
1. a kind of medium temperature phosphate thermosetting resin gelling system, the following components comprising parts by weight meter:
2. medium temperature phosphate thermosetting resin gelling system according to claim 1, the following components comprising parts by weight meter:
3. medium temperature phosphate thermosetting resin gelling system according to claim 1 or 2, it is characterised in that:
The thermosetting resin is selected from least one of melamine resin, furane resins, epoxy resin.
4. medium temperature phosphate 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 aliphatic category, esters, sulfonic acid and Sulfonates.
5. medium temperature phosphate thermosetting resin gelling system according to claim 1 or 2, it is characterised in that:
The phosphate is selected from least one of phosphoric acid, potassium dihydrogen phosphate, sodium dihydrogen phosphate, ammonium dihydrogen phosphate, Quadrafos.
6. medium temperature phosphate thermosetting resin gelling system according to claim 1 or 2, it is characterised in that:
The metal oxide is selected from least one of dead burned magnesia, calcium oxide, aluminium oxide.
7. medium temperature phosphate thermosetting resin gelling system according to claim 1 or 2, it is characterised in that:
The retarder is selected from least one of citrate, boric acid, borax.
8. medium temperature phosphate 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, cellulose family, lignin fluid loss agent.
9. medium temperature phosphate thermosetting resin gelling system according to claim 1 or 2, it is characterised in that:
The lightening material or weighting material are selected from least one of glass microballoon, silicon powder, Iron Ore Powder, modified pitch.
10. the preparation method of described in any item medium temperature phosphate thermosetting resin gelling systems according to claim 1~9,
Be characterized in that the following steps are included:
Each component is weighed up by the dosage first spare；Secondly metal oxide, lightening material or weighting material are uniformly mixed
It mixes to obtain mixed powder；It is again that phosphate, thermosetting resin, resin curing agent, retarder, fluid loss agent, mixing of fresh water is uniform
Obtain mixing liquid；Finally mixed powder is added in mixing liquid under stiring, stirs evenly and obtains the medium temperature phosphoric acid
Salt thermosetting resin gelling system.
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Application publication date: 20190514 |