CN104559974B - A kind of drilling well organic synthesis flexible fragment sealing agent and its preparation method and application - Google Patents
A kind of drilling well organic synthesis flexible fragment sealing agent and its preparation method and application Download PDFInfo
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- CN104559974B CN104559974B CN201410808720.0A CN201410808720A CN104559974B CN 104559974 B CN104559974 B CN 104559974B CN 201410808720 A CN201410808720 A CN 201410808720A CN 104559974 B CN104559974 B CN 104559974B
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- diisocyanate
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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
- C09K8/426—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells for plugging
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/4009—Two or more macromolecular compounds not provided for in one single group of groups C08G18/42 - C08G18/64
- C08G18/4045—Mixtures of compounds of group C08G18/58 with other macromolecular compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
- C08G18/72—Polyisocyanates or polyisothiocyanates
- C08G18/74—Polyisocyanates or polyisothiocyanates cyclic
- C08G18/76—Polyisocyanates or polyisothiocyanates cyclic aromatic
- C08G18/7614—Polyisocyanates or polyisothiocyanates cyclic aromatic containing only one aromatic ring
Abstract
The invention discloses a kind of drilling well organic synthesis flexible fragment sealing agent and its preparation method and application, belong to the organic synthesis flexible fragment sealing agent field in drilling technology field, sealing agent is by gas phase SiO2With nanometer α Al2O3In one or more be modified filler, the diisocyanate of toluene 2,4 and PEG400 copolymer grafted modified bisphenol A type epoxy resin are formed, and the flexible fragment magnitude range is 0.3~13mm, 1.2~2.0g/cm of density3, heatproof >=120 DEG C, alkaline-resisting pH >=12.5, blocking ability >=16.5MPa, filter loss≤500ml.The present invention can be uniformly scattered in the leak stopping slurry of the various density of scene utilization, adapted to the complicated harsh environment in underground, as leak stopping flexible fragment, coordinated leak stopping particle and plugging fiber to go deep into drop ply and be effectively formed bridge joint leak stopping.
Description
Technical field
The invention belongs to the organic synthesis flexible fragment sealing agent field in drilling technology field.
Background technology
In petroleum industry drilling process, leakage can be often met with, leakage can not only extend drilling period, lose a large amount of people
Power material resources, cause formation damage, and leakage once control it is ineffective, it is also possible to the major accidents such as well slough, blowout are induced, so stifled
Leakage material is essential material during drilling well leak-proof leak-stopping.
With Exploration of Oil And Gas, exploitation go deep into, conventional gas and oil resource is fewer and fewer, drilling engineering progressively move towards depth
Layer, ultra deep and deep water, pressure exhaustion stratum and bad ground, circulation problems are more protruded, and are constrained safe, fast, efficient
Drilling well.This just loss circulation material high with greater need for universality strong, excellent performance, disposable leak stopping success rate is developed.
Conventional loss circulation material can be divided into six classes according to the mechanism of action, that is, bridge loss circulation material, high dehydration loss circulation material,
Material, chemical plugging material, inorganic gel loss circulation material and soft (hard) plug class loss circulation material are temporarily blocked up, and bridges loss circulation material and stifled
Leakage technique is at present in practice using most.
Bridge joint loss circulation material can divide three major types in shape：Granular material, fibrous material and flaky material.Wherein piece
Shape material has mica sheet, shell, rice husk, fish scale, broken plastic sheet etc..They mainly play wad act in Process of Leaking Stoppage, therefore
Also known as " tamping ".
" venturi " that granular materials in bridge joint loss circulation material is stuck in leakage channel in Process of Leaking Stoppage serves " bridge formation "；
And flaky material mainly plays wad act, to original gap in the small duct and stratum in " bridge formation " under differential pressure action
It is embedded in and is blocked, further eliminates leakage；Fiber is crisscross in blocking, mutually pull.Three kinds of material synergies,
It is finally reached the purpose of leak stopping.
At present there are various defects in the flaky material sealing agent both at home and abroad employed in petroleum industry drilling engineering, and absolutely
Most of is natural material.
The defect of existing flaky material sealing agent：
1. density is not suitable for：It can not be uniformly dispersed in the leak stopping slurry of various density.
2. being difficult under differential pressure action, the deformation of suitable degree needed for occurring forms effectively closure：It is not easily accessible drop ply,
It is more easy to be blocked in face of hole crack, causes the successful illusion of leak stopping of " sealing up a door "；Even if embedded crack, because formation fracture is
It is irregular, if loss circulation material is hard brittle, its can only shallow-layer closure, plugged zone is easily broken in later stage drillng operation
It is bad, cause former leak source to leak again.
3. the complicated harsh environment of underground can not be adapted to：Such as hygroscopic (oil), easily drop is swelled under high-temperature and high-pressure conditions
Solution, the plugged zone of formation is through after a period of time, intensity can slowly weaken under bottom hole temperature (BHT), pressure, and bearing capacity is reduced, most
Cause plugged zone to fail eventually, cause former leak source to leak again.
The content of the invention
It is an object of the invention to：Propose a kind of drilling well organic synthesis flexible fragment sealing agent and preparation method thereof and answer
With, it can uniformly be scattered in the leak stopping slurry of the live various density used, adapt to the complicated harsh environment in underground, it is deep to leak
Layer is effectively formed bridge joint leak stopping.
The object of the invention is realized by following technical proposals：
The organic synthesis flexible fragment sealing agent in a kind of oil drilling leak stopping field, by gas phase SiO2With nanometer α-Al2O3In
One or more be modified filler, Toluene-2,4-diisocyanate, 4- diisocyanate and PEG400 copolymer grafted modified bisphenol A type epoxy
Resin is formed, and the flexible fragment magnitude range is 0.3~13mm, 1.2~2.0g/cm of density3, heatproof >=120 DEG C, alkaline-resisting pH >=
12.5, blocking ability >=16.5MPa, filter loss≤500ml.
The preparation method of foregoing drilling well organic synthesis flexible fragment sealing agent, by Toluene-2,4-diisocyanate, 4- diisocyanate (TDI)
It is put in reactor, under drying nitrogen protection and quick stirring, PEG400 (polyethylene glycol 400) is at the uniform velocity added dropwise from liquid-feeding tube
In reactor, 45 ± 5min is dripped off, and controlling reaction temperature reacts 4h at 80 ± 3 DEG C, and (TDI and PEG400 mass ratio are 4：
5) bisphenol A type epoxy resin (EP) (TDI and PEG400 gross mass account for the 15% of EP mass), reaction temperature control, are then added
System makees catalyst, stirring reaction 2h is subsequently added into gas phase SiO at 80 ± 3 DEG C with dibutyl tin laurate (DBT-DL)2With
Nanometer α-Al2O3In one or more (content accounts for the 2%~10% of mixture gross mass), first with scattered 20min at a high speed, then
Disperse 15min with supersonic oscillations, make gas phase SiO2Particle sufficiently and uniformly disperses, and is eventually adding methyl tetrahydrochysene O-phthalic
Acid anhydrides (MeTHPA) is curing agent, and 2,4,6-three (dimethylamino methyl) phenol (DMP-30) do accelerator, and quick stirring is equal
It is even, in the mould that preheating is poured into after vacuum defoamation, solidify 24h at 120 ± 3 DEG C, be finally stripped, crushing.
The application of foregoing drilling well organic synthesis flexible fragment sealing agent, as leak stopping flexible fragment, coordinates leak stopping particle
Bridge joint leak stopping is applied to plugging fiber.
The present invention is by introducing flexible side-chains and gas phase SiO2, nanometer α-Al2O3Epoxy resin is modified, can
The need for adapting to underground leak stopping.
Principal product：
WhereinRepresent
By introducing flexible side-chains in EP, make its flexibility increase.
Before principal product solidification, by gas phase SiO2, nanometer α-Al2O3Rear ultrasonic wave is disperseed by first exceeding the speed limit for special time
Dispersing mode is by its " insertion " resin, and because its size is small, specific surface area is big, and the coordination of surface seriously is not enough, and surface
Oxygen debt the features such as, it is set to show extremely strong activity, and the oxygen of epoxy ring molecule plays bonding action, improves intermolecular key
Power, with some Nano-meter SiO_2 of fashion2, nanometer α-Al2O3Particle is still distributed in the space of macromolecular chain, so that epoxy
Resin material meets leak stopping needs.
Product before modified after mechanical property：
Product before modified after mechanical property
Beneficial effects of the present invention：
1. by introducing flexible side-chains and addition gas phase SiO to epoxy resin2, nanometer α-Al2O3It is modified, in high temperature
Down-hole liquid environment in it is not degradable.
2. products made thereby of the present invention can be uniformly scattered in leak stopping slurry, overcoming conventional natural flake material can not
It is uniformly dispersed in the practical problem in leak stopping slurry.
3. products made thereby of the present invention is in leak stopping under differential pressure action, the flexible leak stoppage piece with face when contacting formation fracture
It is foldable or deform into fracture plugging, it is to avoid as traditional hard fragility sheet loss circulation material to produce " closure door " leak stopping successfully
Illusion；When touch meet irregular cracks when, the invention, which can be deformed upon, gos deep into fracture plugging, it is to avoid traditional hard fragility sheet is blocked up
Leakage material is only capable of shallow-layer closure, blocks not firm enough, is spudded in again after leak stopping when causing pressure oscillation, the tamper at place is blocked up
It can disengage, occur the situation of leakage again.
4. products made thereby of the present invention has materialization inertia, do not absorb water (oil), with resistant to elevated temperatures performance, it is ensured that in underground still
With enough intensity, gap or the formation fracture of granular material can be firmly clogged, without as natural plants sheet
Loss circulation material is swelled degraded under high temperature soaking conditionses, ultimately results in plugged zone failure, causes former leak source to leak again.
5. products made thereby of the present invention can deeply be clogged in folded deformation under differential pressure action bridge formation granular materials gap or
Formation fracture, can greatly improve the bearing capacity of drop ply.
Embodiment
Following non-limiting examples are used to illustrate the present invention.
Embodiment 1：
Following ingredients are by weight ratio：40 parts of Toluene-2,4-diisocyanates are taken, 4- diisocyanate (TDI) is put in reactor,
Under drying nitrogen protection and quick stirring, 50 parts of polyethylene glycol 400s (PEG400) are at the uniform velocity added dropwise from liquid-feeding tube in reactor,
45 ± 5min is dripped off, and controlling reaction temperature reacts 4h at 80 ± 3 DEG C.Then 600 parts of bisphenol A type epoxy resins (EP) are added, instead
Temperature control is answered at 80 ± 3 DEG C, catalyst is made with dibutyl tin laurate (DBT-DL), stirring reaction 2h is subsequently added into
13.8 parts of gas phase SiO2, first with scattered 20min at a high speed, then with the scattered 15min of supersonic oscillations, make gas phase SiO2Particle is fully,
Disperse evenly.Methyl tetrahydrophthalic anhydride (MeTHPA) is eventually adding for curing agent, 2,4,6-three (dimethylamino methyls)
Phenol (DMP -30) does accelerator, quickly stirs, in the mould that preheating is poured into after vacuum defoamation, solid at 120 ± 3 DEG C
Change 24h.The demoulding, crushing.Product flexible fragment size is 0.3~13mm, density 1.22g/cm3, in 120 DEG C of pH value 12.5
Sodium hydroxide solution in mass loss rate 15.48%, blocking ability >=16.5MPa, filter loss 446ml.
Note：Raw material and product used herein are commercially available technical grade.
The testing standard or method of aforementioned data are as follows：
The alkaline-resisting detection method of heatproof：Weigh sample 10g (being accurate to 0.01g) and be designated as m, be put into high temperature ageing tank, then add
Enter the sodium hydroxide solution that 350ml pH are 12.5, be put into high temp roller heating furnace after good seal small in aging 16 at 120 DEG C
When after cooling, can opening, washed samples to non-alkali liquor remain after, at 105 DEG C dry, in drier cool down after weigh, be designated as
m1.Mass loss rateS≤20% is considered as 120 DEG C of heatproof, resistance to pH value 12.5.
Blocking ability, leakage quantity measuring method：Base is starched：5000ml distilled water is measured, under electric mixer stirring condition
Bentonite 370g, sodium carbonate 2g are added, adds up stirring 1h, closed placement 16h is standby at room temperature.Base slurry apparent viscosity should be
16mPas~22mPas.Experiment slurry：Take 3000ml bases to starch, add sample 12g, organic synthesis leak stopping particle (such as filler
Such as calcium carbonate crystal whisker, magnesium borate crystal whisker and calcium carbonate crystal whisker reinforced polyether ether ketone/PEI) 580g (0.550mm~
1.000mm200g, 1.000mm~1.700mm200g, 1.700mm~2.800mm60g, 2.800mm~4.000mm60g,
3.350mm~4.750mm60g), (such as aerosil, activated Calcium carbonate and titanium dioxide etc. fill organic synthesis alloy fiber
The polyether sulfone filled out/polytetrafluoroethylblended blended thing) 12g, while adding 150g drill-feeding plugging agents, 30min is stirred, 30min is stood, then
5min is stirred, as experiment slurry.14mm steel balls 400g, 10mm steel ball 400g, 4mm steel ball 600g is weighed respectively, by alleged steel ball
It is placed in the steel ball bed of device for plugging configuration and (first puts small, amplify afterwards), steel ball is shaken up and is put into after paving in device for plugging
In chamber.In the experiment slurry injection loss circulation material device that 3000ml is prepared, cover is screwed, pressurized pipeline is connected, 5min is stood.
Floss hole is opened, source of the gas is opened and pressurizes, first add 0.7MPa pressure, is increased after collecting experiment slurry wastage, stabilization at interval of 2min
0.5MPa pressure, until pressure is increased into 16.5MPa, voltage stabilizing 30min, reads total experiment slurry wastage.If pressure is increased
Filter loss≤500ml after voltage stabilizing 30min, that is, be considered as blocking ability >=16.5MPa under to 16.5MPa.
Embodiment 2：
The present embodiment is substantially the same manner as Example 1, and its difference is：By 13.8 parts of gas phase SiO in embodiment 12Change into
Nanometer α-Al2O3.Product flexible fragment size is 0.3~13mm, density 1.37g/cm3, in the hydroxide of 120 DEG C of pH value 12.5
Mass loss rate 14.87% in sodium solution, blocking ability >=16.5MPa, filter loss 463ml.Experiment detection method is as described above.
Embodiment 3：
The present embodiment is substantially the same manner as Example 1, and its difference is：By 13.8 parts of gas phase SiO in embodiment 12Change into
69 parts of gas phase SiO2.Product flexible fragment size is 0.3~13mm, density 1.82g/cm3, in the hydroxide of 120 DEG C of pH value 12.5
Mass loss rate 16.91% in sodium solution, blocking ability >=16.5MPa, filter loss 450ml.Experiment detection method is as described above.
Embodiment 4：
The present embodiment is substantially the same manner as Example 1, and its difference is：By 13.8 parts of gas phase SiO in embodiment 12Change into
69 parts of nanometer α-Al2O3.Product flexible fragment size is 0.3~13mm, density 1.96g/cm3, in the hydrogen of 120 DEG C of pH value 12.5
Mass loss rate 17.88% in sodium hydroxide solution, blocking ability >=16.5MPa, filter loss 478ml.Experiment detection method is as above
It is described.
Embodiment 5：
The present embodiment is substantially the same manner as Example 1, and its difference is：By 13.8 parts of gas phase SiO in embodiment 12Change into
20 parts of gas phase SiO2With 30 parts of nanometer α-Al2O3.Product flexible fragment size is 0.3~13mm, density 1.59g/cm3, 120
Mass loss rate 15.30%, blocking ability >=16.5MPa, filter loss 485ml in the sodium hydroxide solution of DEG C pH value 12.5.It is real
Test detection method as described above.
Embodiment 6：
The present embodiment is substantially the same manner as Example 1, and its difference is：By 13.8 parts of gas phase SiO in embodiment 12Change into
30 parts of gas phase SiO2With 20 parts of nanometer α-Al2O3.Product flexible fragment size is 0.3~13mm, density 1.51g/cm3, 120
Mass loss rate 13.08%, blocking ability >=16.5MPa, filter loss 477ml in the sodium hydroxide solution of DEG C pH value 12.5.It is real
Test detection method as described above.
Comparative example 1：
Unmodified bisphenol A type epoxy resin：Density 1.16g/cm3, the quality in the soda bath of 120 DEG C of pH value 12.5
Loss late 48.06%.Test method be the same as Example 1.
Comparative example 2：
This comparative example is substantially the same manner as Example 1, and its difference is：By Toluene-2,4-diisocyanate in embodiment 1,4- diisocyanate by
40 parts change 50 parts into.Product chip size is 0.3~13mm, density 1.32g/cm3, in the sodium hydroxide of 120 DEG C of pH value 12.5
Mass loss rate 30.58% in solution, experiment detection method is as described above.
Comparative example 3：
This comparative example is substantially the same manner as Example 1, and its difference is：Polyethylene glycol 400 in embodiment 1 is changed into by 50 parts
60 parts.Product chip size is 0.3~13mm, density 1.17g/cm3, the matter in the sodium hydroxide solution of 120 DEG C of pH value 12.5
Amount loss rate 23.58%, experiment detection method is as described above.
Comparative example 4：
This comparative example is substantially the same manner as Example 1, and its difference is：By bisphenol A type epoxy resin dosage in embodiment 1 by
600 parts change 700 parts into.Product chip size is 0.3~13mm, density 1.20g/cm3, in the hydroxide of 120 DEG C of pH value 12.5
Mass loss rate 25.10% in sodium solution, experiment detection method is as described above.
Comparative example 5：
This comparative example is substantially the same manner as Example 1, and its difference is：By bisphenol A type epoxy resin in embodiment 1 by 600
Part changes 500 parts into.Product chip size is 0.3~13mm, density 1.25g/cm3, it is molten in the sodium hydroxide of 120 DEG C of pH value 12.5
Mass loss rate 29.22% in liquid, experiment detection method is as described above.
Comparative example 6：
This comparative example is substantially the same manner as Example 1, and its difference is：By gas phase SiO in embodiment 12Changed into by 13.8 parts
10 parts.Product chip size is 0.3~13mm, density 1.18g/cm3, the matter in the sodium hydroxide solution of 120 DEG C of pH value 12.5
Amount loss rate 25.50%, experiment detection method is as described above.
Comparative example 7：
This comparative example is substantially the same manner as Example 1, and its difference is：By 13.8 parts of gas phase SiO in embodiment 12Change 10 into
Part nanometer α-Al2O3.Product chip size is 0.3~13mm, density 1.20g/cm3, in the sodium hydroxide of 120 DEG C of pH value 12.5
Mass loss rate 28.48% in solution, experiment detection method is as described above.
Comparative example 8：
This comparative example is substantially the same manner as Example 1, and its difference is：By gas phase SiO in embodiment 12Changed into by 13.8 parts
72 parts.Product chip size is 0.3~13mm, density 1.85g/cm3, the matter in the sodium hydroxide solution of 120 DEG C of pH value 12.5
Amount loss rate 27.17%, experiment detection method is as described above.
Comparative example 8：
This comparative example is substantially the same manner as Example 1, and its difference is：By 13.8 parts of gas phase SiO in embodiment 12Change 72 into
Part nanometer α-Al2O3.Product chip size is 0.3~13mm, density 1.98g/cm3, in the sodium hydroxide of 120 DEG C of pH value 12.5
Mass loss rate 24.03% in solution, experiment detection method is as described above.
Comparative example 9：
Common broken plastic sheet (polyethylene terephthalate class)：Density 1.40g/cm3, in 120 DEG C of pH value 12.5
Mass loss rate 14.21% in soda bath, blocking ability ＜ 16.5MPa, filter loss 879ml.Test method be the same as Example 1.
Comparative example 10：
Common broken plastic sheet (PP type)：Density 0.91g/cm3, density is too low, and fraction floats starch top in leak stopping, point
Dissipate inequality.The mass loss rate 15.18% in the soda bath of 120 DEG C of pH value 12.5, but deformation is serious before and after heat rolling.Experiment
Method be the same as Example 1.
Comparative example 11：
Mica sheet：Density 2.73g/cm3Density, density is too high, is partly sunken to and starches bottom in leak stopping, disperses inequality.120
Mass loss rate 30.12%, blocking ability ＜ 16.5MPa, filter loss 1157ml in the soda bath of DEG C pH value 12.5.Experiment side
Method be the same as Example 1.
Comparative example 12：
This comparative example is substantially the same manner as Example 1, and its difference is：Without modified filler, product chip size is 0.3~
13mm, density 1.21g/cm3, the mass loss rate 26.31% in the soda bath of 120 DEG C of pH value 12.5.Test method is with real
Apply example 1.
Comparative example 13：
This comparative example is substantially the same manner as Example 1, and its difference is：By 13.8 parts of gas phase SiO in embodiment 12By changing into
Nano-TiO2.Product chip size is 0.3~13mm, density 1.38g/cm3, in the sodium hydroxide solution of 120 DEG C of pH value 12.5
Mass loss rate 30.72%, test method be the same as Example 1.
Comparative example 14：
This comparative example is substantially the same manner as Example 1, and its difference is：By 13.8 parts of gas phase SiO in embodiment 12By changing into
Ultra-fine CaCO3.Product chip size is 0.3~13mm, density 1.20g/cm3, in the sodium hydroxide solution of 120 DEG C of pH value 12.5
Middle mass loss rate 41.72%, test method be the same as Example 1.
Contrast is summarized：
By above-mentioned strict, sufficient comparative example, the specific parameter selection of the present invention achieves significant effect and carried
Rise.Various conventional selections of the those skilled in the art outside the scope of claim all do not reach the effect of the present invention far.
Wherein, comparative example 1 is only pure bisphenol A type epoxy resin, and comparative example 9 is pure polyethylene terephthalate class,
Comparative example 10 is virgin pp class；Comparative example 2-8 is the component proportion of non-invention, is non-filling mixture ratio, non-polymer respectively
Proportioning, non-polymer and filling mixture ratio；Comparative example 11 is existing conventional mica sheet loss circulation material；Comparative example 12 is the poly- of the present invention
Compound is not added with filler；Comparative example 13,14 adds other fillers for the polymer of the present invention.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
Any modifications, equivalent substitutions and improvements made within refreshing and principle etc., should be included in the scope of the protection.
Claims (3)
1. a kind of drilling well organic synthesis flexible fragment sealing agent, it is characterised in that：By gas phase SiO2With nanometer α-Al2O3In
One or more are modified filler, Toluene-2,4-diisocyanate, 4- diisocyanate and PEG400 copolymer grafted modified bisphenol A type asphalt mixtures modified by epoxy resin
Fat is formed, and the flexible fragment magnitude range is 0.3~13mm, 1.2~2.0g/cm of density3, heatproof >=120 DEG C, alkaline-resisting pH >=
12.5, blocking ability >=16.5MPa, filter loss≤500ml.
2. the drilling well as claimed in claim 1 preparation method of organic synthesis flexible fragment sealing agent, it is characterised in that：By first
Benzene -2,4- diisocyanate is put in reactor, under drying nitrogen protection and quick stirring, is at the uniform velocity added dropwise from liquid-feeding tube
PEG400 is in reactor, Toluene-2,4-diisocyanate, and 4- diisocyanate and PEG400 mass ratio are 4：5,45 ± 5min is dripped off, and control is anti-
Temperature is answered to react 4h at 80 ± 3 DEG C；Then bisphenol A type epoxy resin, and Toluene-2,4-diisocyanate are added, 4- diisocyanate and PEG400's
Gross mass accounts for the 15% of bisphenol A type epoxy resin quality, and reaction temperature is controlled at 80 ± 3 DEG C, made with dibutyl tin laurate
Catalyst, stirring reaction 2h is subsequently added into gas phase SiO2With nanometer α-Al2O3In one or more, it is total that its content accounts for mixture
The 2%~10% of quality, first with scattered 20min at a high speed, then with the scattered 15min of supersonic oscillations, makes gas phase SiO2Particle fully,
It is uniformly dispersed, is eventually adding methyl tetrahydrophthalic anhydride for curing agent, 2,4,6-three (dimethylamino methyl) phenol are done
Accelerator, quickly stirs, in the mould that preheating is poured into after vacuum defoamation, solidifies 24h at 120 ± 3 DEG C, is finally stripped,
Crushing.
3. the drilling well as claimed in claim 1 application of organic synthesis flexible fragment sealing agent, it is characterised in that：It is used as leak stopping
Flexible fragment, coordinates leak stopping particle and plugging fiber to be applied to bridge joint leak stopping.
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| CN109575570A (en) * | 2018-12-06 | 2019-04-05 | 镇江利德尔复合材料有限公司 | A kind of preparation method of the excellent polyurethane material of novel shape-memory properties |
| CN109869115A (en) * | 2019-01-22 | 2019-06-11 | 中国石油天然气股份有限公司长庆油田分公司第六采油厂 | A method of slug is sealed using titanate system solution |
| CN110144035A (en) * | 2019-05-24 | 2019-08-20 | 桂林电子科技大学 | A kind of polyethylene glycol Graft Epoxy Resin composite material and preparation method |
| CN110437408B (en) * | 2019-07-19 | 2021-07-23 | 中国石油集团川庆钻探工程有限公司 | Curing agent for high-temperature excitation type oil-based drilling fluid and preparation method thereof |
| CN111440348B (en) * | 2020-04-13 | 2022-05-03 | 江苏鼎峰石油科技有限公司 | Preparation method of flake-type high-temperature-resistant self-suspending plugging agent |
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| CN102408860B (en) * | 2011-10-19 | 2013-03-06 | 湖南固特邦土木技术发展有限公司 | Flexible epoxy adhesive and application |
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