CN110117485A - A kind of highdensity epoxy resin plugging material - Google Patents
A kind of highdensity epoxy resin plugging material Download PDFInfo
- Publication number
- CN110117485A CN110117485A CN201910382111.6A CN201910382111A CN110117485A CN 110117485 A CN110117485 A CN 110117485A CN 201910382111 A CN201910382111 A CN 201910382111A CN 110117485 A CN110117485 A CN 110117485A
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- epoxy resin
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- quartz sand
- bisphenol
- plugging material
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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
- C09K8/44—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells containing organic binders only
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- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Epoxy Resins (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
A kind of highdensity epoxy resin plugging material.The plugging material is to mix quartz sand with bisphenol f type epoxy resin, polyfunctional epoxy resin etc. after titanate coupling agent pre-processes, and adjusts density with quartz sand, controls curing reaction by polyfunctional epoxy resin, solidifies at 80 DEG C.65~92MPa of plugging material compression strength prepared by the present invention, density are 1.21~1.43g/cm3, oil/gas well can effectively be blocked.Solidfied material is free of harmful volatile matter, is conducive to environmental protection.
Description
Technical field
The present invention relates to a kind of oil/gas well plugging materials, furtherly, are related to a kind of highdensity epoxy resin closure
Material.
Background technique
In oil gas well cementing operation link, cement sheath plays the role of blocking subterranean fracture layer, prevents crossflow.But it seals
The stifled long-time stability that not exclusively will affect cement sheath, reduce its mechanical property, therefore fracture layer is needed to be blocked, asphalt mixtures modified by epoxy resin
Rouge is the novel plugging material after well cementing of cement.CN107216609A is related to a kind of fast blockage epoxide resin grouting material,
Main component is 40 parts of epoxy resin E-51 and 60 parts of epoxy resin E-44s, 10~20 parts of benzyl glycidyl ethers, 30~40 parts
Curing agent, the density of mixing post-grouting material are 1.11g/cm3, compression strength is 83.5~87.5MPa, can be consolidated at normal temperature
Change.
Hole condition is had nothing in common with each other when oil/gas well blocks operation, and density needed for influence of the different regions because of factors such as water, oil is different,
For the stability for ensureing material in transmission process, the density of plugging material is adjusted by inorganic filler, it is made to meet different well's conditions
Demand.CN105694796A discloses a kind of polyurethane clay, and main component is 50~100 parts of polyurethane modified epoxy trees
Rouge, 7.5~22.5 parts of granularities are lower than mica powder, 85~275 parts of Al of 200 mesh2O3, the clay density of preparation is 2.0g/cm3Gu
Compression strength is 70MPa after change, can prevent the extension of crackle.CN105001596A discloses a kind of closure material of well cementing operation
Material, main component are 75 parts of bisphenol f type epoxy resin NPEL-128,100 parts of manganese mineral powders, 1 part of fumed silica, serum density
For 1.8g/cm3, compression strength 43MPa after solidification, can prevent gas well exploit in wellheadpressure phenomenon generation.
CN108865087A discloses a kind of thermosetting epoxy resin anchorage liquid, and main component is 100 parts of aqueous epoxy resins, 30
Part barite, 40 parts of Iron Ore Powders, 1~30 part of water, having prepared density after each component mixing is respectively 1.30g/cm3And 1.45g/
cm3Working solution, 50 DEG C solidification after compression strength be respectively 22.0MPa and 19.6MPa, intensity is lower.
A kind of highdensity epoxy resin plugging material of invention, quartz sand is after titanate coupling agent pre-processes
It mixing with bisphenol f type epoxy resin, polyfunctional epoxy resin etc., solidifies at 80 DEG C, the density of material prepared is 1.21~
1.43g/cm3, compression strength is 65~92MPa.
Summary of the invention
The purpose of the present invention is to provide a kind of highdensity epoxy resin plugging materials.The plugging material is by quartz sand
It mixes, is adjusted with quartz sand close with bisphenol f type epoxy resin, polyfunctional epoxy resin etc. after titanate coupling agent pre-processes
Degree controls curing reaction by polyfunctional epoxy resin, solidifies at 80 DEG C, and plugging material compression strength prepared by the present invention 65~
92MPa, density are 1.21~1.43g/cm3, oil/gas well can effectively be blocked.
The technical solution of the present invention is as follows:
A kind of highdensity epoxy resin plugging material, raw material include bisphenol f type epoxy resin, polyfunctional epoxy resin,
Diluent, curing agent, promotor, titanate coupling agent and quartz sand, raw material proportioning are as follows:
The bisphenol f type epoxy resin is one in bisphenol f type epoxy resin YDF-165, YDF-2001, YDF-161H
Kind is several, and the polyfunctional epoxy resin is four glycidyl ether tetraphenyl ethane, trisphenyl glycidyl ether Ji Jia
Alkane, four glycidyl group dimethylphenylene diamine, triglycidyl group-P- amino-phenol, four glycidyl group diamino dimethylene
One or more of benzene.
The diluent is 1,4-butanediol diglycidyl ether, ethylene glycol diglycidylether, butyl glycidyl
One or more of ether, 4,4 '-diamino-dicyclohexyl methane of curing agent, 3,3 '-dimethyl -4,4 '-diamino, two ring
One or more of hexyl methane, modified by cardanol phenolic aldehyde amine, promotor 2,4,6- tri- (dimethylamino methyl) phenol, titanium
Acid esters coupling agent is isopropyl three (dioctylphyrophosphoric acid acyloxy) titanate esters.
The quartz sand size is 2400 mesh, density 2.45g/cm3, isopropyl three is used before use, and (dioctyl is burnt
Phosphoric acid acyloxy) titanate coupling agent pretreatment.
The preparation method of the plugging material, includes the following steps:
(1) 1.2~1.5 parts of isopropyls three (dioctylphyrophosphoric acid acyloxy) titanate esters and 50ml ethanol water (1 are weighed
: 9) it is placed in three-neck flask, is quickly stirred at 30~60 DEG C with the speed of 3000rpm, when stirring is slowly added to 10~25 parts
Quartz sand simultaneously stirs 30~60min, and it is stand-by with distilled water washing to be placed in 100 DEG C of baking oven dry 3h after the completion of stirring；
It (2) at room temperature, will be at 100 parts of bisphenol f type epoxy resins, 2~8 parts of polyfunctional epoxy resins, 10~25 parts of couplings
Quartz sand and 20~35 parts of diluents after reason stir evenly in agitator tank, stand 5min；
(3) 20~25 parts of curing agent, 0.7~2 part of promotor are added into agitator tank, stir evenly, in vacuum oven
Bubble is eliminated, is then being poured in a mold；
(4) casting material is solidified for 24 hours at 80 DEG C.
The beneficial effects of the present invention are:
(1) wetability that titanate coupling agent treated quartz sand and material are asked improves, and improves quartz sand in material
Middle stability, is uniformly distributed quartz sand in material.The density of the highdensity epoxy resin plugging material of the present invention is 1.21
~1.43g/cm3, the closure operation under different well's conditions can be met.
(2) bisphenol f type epoxy resin, polyfunctional epoxy resin are used in mixed way the crosslink density for improving and blocking material, make to seal
The compression strength of putty improves.The highdensity epoxy resin plugging material intensity of the present invention is high, the pressure resistance of pour mass after solidification
Degree is up to 92MPa.
(3) solidfied material is free of harmful volatile matter, is conducive to environmental protection.
Specific embodiment
It is further illustrated below with reference to example:
Embodiment one
Weigh 1.2 parts of isopropyls three (dioctylphyrophosphoric acid acyloxy) titanate coupling agent and 50ml ethanol water (1:
9) it is placed in three-neck flask, is quickly stirred at 40 DEG C with the speed of 3000rpm, after when stirring is slowly added to 10 parts of coupling processings
Quartz sand simultaneously stirs 30min, and it is stand-by with distilled water washing to be placed in 100 DEG C of baking oven dry 3h after the completion of stirring.
At room temperature, 100 parts of epoxy resin YDF-165,8 part of four glycidyl ether tetraphenyl ethane, 10 parts of coupling processings
Quartz sand and 25 parts of 1,4-butanediol diglycidyl ether afterwards is added in agitator tank and is stirred evenly, and stands 5min；To agitator tank
Middle to be added 20 part 4,4 '-diamino-dicyclohexyl methanes, 1.0 part 2,4,6- tri- (dimethylamino methyl) phenol stir evenly, very
Bubble is eliminated in empty drying box, is then being poured in a mold；Casting material is solidified for 24 hours at 80 DEG C.
Viscosity: measuring method measures the initial viscosity of material referring to GB 2794-81 at room temperature.
Density: measuring method is referring to GB/T 6343-2009, the density of pour mass after measurement solidifies at room temperature.
Compression strength and elasticity modulus: measuring method measures at room temperature referring to GB/T2567-2008.
Embodiment two
Implementation steps with example one, the difference is that: isopropyl three (dioctylphyrophosphoric acid acyloxy) titanate coupling agent
Becoming 1.5 parts from 1.2 parts, mixing time becomes 60min from 30min, and the quartz sand after coupling processing becomes 15 parts from 10 parts, and four
Glycidyl ether tetraphenyl ethane replaces with trisphenyl glycidyl ether methylmethane, 2,4,6- tri- (dimethylamino methyl) phenol
Become 1.3 parts from 1.0 parts.
Performance measurement: method is the same as embodiment one.
Embodiment three
Implementation steps with example one, the difference is that: whipping temp becomes 60 DEG C from 30 DEG C, the quartz sand after coupling processing
20 parts are changed to by 10 parts, 25 parts of 1,4-butanediol diglycidyl ether replace with 32 parts of butyl glycidyl ethers, and 20 part 4,4 '-two
Amino bicyclic hexyl methane replaces with 25 parts of modified by cardanol phenolic aldehyde amines.
Performance measurement: method is the same as embodiment one.
Example IV
Implementation steps with example one, the difference is that: isopropyl three (dioctylphyrophosphoric acid acyloxy) titanate coupling agent
Becoming 1.5 parts from 1.2 parts, mixing time becomes 60min from 30min, and the quartz sand after coupling processing becomes 25 parts from 10 parts, and 8
Part four glycidyl ether tetraphenyl ethane are changed to 5 parts of trisphenyl glycidyl ether methylmethanes, and 20 part 4,4 '-diamino, two hexamethylene
Methylmethane replaces with 25 parts of modified by cardanol phenolic aldehyde amines, and 2,4,6- tri- (dimethylamino methyl) phenol are changed to 1.8 parts by 1.0.
Performance measurement: method is the same as embodiment one.
The property and performance of the highdensity epoxy resin plugging material of the subordinate list present invention
| Embodiment one | Embodiment two | Embodiment three | Example IV | |
| Initial viscosity/mPas | 743 | 813 | 889 | 947 |
| Density g/cm3 | 1.21 | 1.28 | 1.37 | 1.43 |
| Compression strength/MPa | 65.8 | 78.9 | 91.6 | 81.8 |
| Elasticity modulus/GPa | 1.21 | 1.32 | 2.33 | 2.01 |
The above content is a further detailed description of the present invention in conjunction with specific preferred embodiments, and it cannot be said that
A specific embodiment of the invention is only limitted to this, for those of ordinary skill in the art to which the present invention belongs, is not taking off
Under the premise of from present inventive concept, several simple deduction or replace can also be made, all shall be regarded as belonging to the present invention by institute
Claims of submission determine scope of patent protection.
Unaccomplished matter of the present invention is well-known technique.
Claims (4)
1. a kind of highdensity epoxy resin plugging material, raw material includes bisphenol f type epoxy resin, polyfunctional epoxy resin, dilute
Release agent, curing agent, promotor, titanate coupling agent and quartz sand, raw material proportioning are as follows:
The bisphenol f type epoxy resin be one of bisphenol f type epoxy resin YDF-165, YDF-2001, YDF-161H or
Several, the polyfunctional epoxy resin is four glycidyl ether tetraphenyl ethane, trisphenyl glycidyl ether methylmethane, four
Glycidyl dimethylphenylene diamine, triglycidyl group-P- amino-phenol, in four glycidyl group diamino dimethylene benzene
It is one or more of.
2. diluent as described in claim 1 is 1,4-butanediol diglycidyl ether, ethylene glycol diglycidylether, butyl
One or more of glycidol ether, 4,4 '-diamino-dicyclohexyl methane of curing agent, 3,3 '-dimethyl -4,4 '-two
One or more of amino bicyclic hexyl methane, modified by cardanol phenolic aldehyde amine, promotor 2,4, (the dimethylamino first of 6- tri-
Base) phenol, titanate coupling agent is isopropyl three (dioctylphyrophosphoric acid acyloxy) titanate esters.
3. quartz sand size as described in claim 1 is 2400 mesh, density 2.45g/cm3, isopropyl three is used before use
The pretreatment of (dioctylphyrophosphoric acid acyloxy) titanate coupling agent.
4. the preparation method of plugging material as described in claim 1, includes the following steps:
(1) 1.2~1.5 parts of isopropyls three (dioctylphyrophosphoric acid acyloxy) titanate esters and 50ml ethanol water (1: 9) are weighed
It is placed in three-neck flask, is quickly stirred at 30~60 DEG C with the speed of 3000rpm, when stirring is slowly added to 10~25 parts of quartz
Sand simultaneously stirs 30~60min, and it is stand-by with distilled water washing to be placed in 100 DEG C of baking oven dry 3h after the completion of stirring；
It (2) at room temperature, will be after 100 parts of bisphenol f type epoxy resins, 2~8 parts of polyfunctional epoxy resins, 10~25 parts of coupling processings
Quartz sand and 20~35 parts of diluents stirred evenly in agitator tank, stand 5min；
(3) 20~25 parts of curing agent, 0.7~2 part of promotor are added into agitator tank, stirs evenly, is eliminated in vacuum oven
Then bubble is being poured in a mold；
(4) casting material is solidified for 24 hours at 80 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910382111.6A CN110117485A (en) | 2019-05-06 | 2019-05-06 | A kind of highdensity epoxy resin plugging material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910382111.6A CN110117485A (en) | 2019-05-06 | 2019-05-06 | A kind of highdensity epoxy resin plugging material |
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| Publication Number | Publication Date |
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| CN110117485A true CN110117485A (en) | 2019-08-13 |
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ID=67521961
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| CN201910382111.6A Pending CN110117485A (en) | 2019-05-06 | 2019-05-06 | A kind of highdensity epoxy resin plugging material |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111205837A (en) * | 2020-01-14 | 2020-05-29 | 郑州大学 | Single-component annular plugging agent and application method thereof |
| CN111499532A (en) * | 2020-05-07 | 2020-08-07 | 万华化学集团股份有限公司 | Preparation and application of epoxy resin foaming agent |
| CN111793481A (en) * | 2020-06-12 | 2020-10-20 | 中国石油天然气集团公司 | Resin cementing material for oil-gas well as preparation method and application thereof |
| CN111995995A (en) * | 2020-09-03 | 2020-11-27 | 西南石油大学 | Bulk-expanded particle heterogeneous crack plugging effect improving agent and preparation method thereof |
| CN112341999A (en) * | 2020-10-23 | 2021-02-09 | 安东石油技术（集团）有限公司 | Epoxy resin well cementation plugging system and preparation method and application thereof |
| CN115895613A (en) * | 2021-08-06 | 2023-04-04 | 中国石油天然气集团有限公司 | Temperature-controlled resin cementing and leaking stoppage working solution and preparation method thereof |
-
2019
- 2019-05-06 CN CN201910382111.6A patent/CN110117485A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111205837A (en) * | 2020-01-14 | 2020-05-29 | 郑州大学 | Single-component annular plugging agent and application method thereof |
| CN111499532A (en) * | 2020-05-07 | 2020-08-07 | 万华化学集团股份有限公司 | Preparation and application of epoxy resin foaming agent |
| CN111499532B (en) * | 2020-05-07 | 2022-09-20 | 万华化学集团股份有限公司 | Preparation and application of epoxy resin foaming agent |
| CN111793481A (en) * | 2020-06-12 | 2020-10-20 | 中国石油天然气集团公司 | Resin cementing material for oil-gas well as preparation method and application thereof |
| CN111995995A (en) * | 2020-09-03 | 2020-11-27 | 西南石油大学 | Bulk-expanded particle heterogeneous crack plugging effect improving agent and preparation method thereof |
| CN111995995B (en) * | 2020-09-03 | 2021-04-30 | 西南石油大学 | Bulk-expanded particle heterogeneous crack plugging effect improving agent and preparation method thereof |
| CN112341999A (en) * | 2020-10-23 | 2021-02-09 | 安东石油技术（集团）有限公司 | Epoxy resin well cementation plugging system and preparation method and application thereof |
| CN115895613A (en) * | 2021-08-06 | 2023-04-04 | 中国石油天然气集团有限公司 | Temperature-controlled resin cementing and leaking stoppage working solution and preparation method thereof |
| CN115895613B (en) * | 2021-08-06 | 2024-05-31 | 中国石油天然气集团有限公司 | Temperature-control resin glue-fixing plugging working solution and preparation method thereof |
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Application publication date: 20190813 |