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Dynamic crosslinking degradable epoxy resin and preparation method and high-temperature leaking stoppage application thereof

A dynamic cross-linking, epoxy resin technology, applied in chemical instruments and methods, recycling technology, drilling composition, etc., can solve the problems of reducing mechanical properties, unable to meet the application requirements of high temperature leakage plugging, and achieve leakage protection layer effect

Pending Publication Date: 2022-06-03
CNOOC TIANJIN BRANCH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The introduction of easy-to-break ester bonds, carbamate bonds, carbonates, acetal groups, etc. into the epoxy structure can make it degrade at a lower temperature, but at the same time it also reduces the mechanical properties, which cannot meet high-temperature plugging applications requirements, therefore, this needs to be improved

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Weigh epoxy monomer E51 (50%), curing agent methylhexahydrophthalic anhydride-MHHPA (50%) and auxiliary agent zinc acetylacetonate-Zn(acac) in a beaker respectively 2 (10%), heated and stirred in an oil bath at 100°C, then mixed, poured into a mold, and put into an oven to cure at 100°C for 2 hours, 130°C for 2 hours, and 150°C for 2 hours; the glass transition of the obtained solid product The temperature was 150°C, and the temperature of 5% thermal weight loss was 300°C; the solid product sample was immersed in oil, aged in an oven at 180°C for 10 days, with a mass loss of 8.5%, and aged for 30 days with a mass loss of 80%.

[0038] The solid product was aged in an oven at 180°C for 10 days and 30 days; the unaged solid samples and aged samples were pulverized into particles as a plugging agent, and the plugging agent (8%) was mixed with calcium carbonate particles (15%, wherein , 10~20 mesh calcium carbonate 7%, 20~40 mesh calcium carbonate 4%, 40~80 mesh calcium car...

Embodiment 2

[0040] Same as Example 1, the difference is: the epoxy monomer (57%) adopted is E44 and 4.4-diaminodiphenylmethane tetraglycidylamine-TGDOM, and the curing agent is methylhexahydrophthalic anhydride-MHHPA (43 %), the auxiliary agent is zinc acetate-ZnAD (10%). The heating and curing process is as follows: curing at 60 °C for 1 hour, curing at 100 °C for 1 hour, curing at 130 °C for 2 hours, and curing at 150 °C for 2 hours.

[0041] The glass transition temperature of the solid product obtained in this example is 179°C, and the temperature at which 5% thermal weight loss occurs is 320°C; the solid product sample is immersed in oil, aged in an oven at 180°C for 10 days, with a mass loss of 4.5%, and aged for 30 days , with a mass loss of 73%.

[0042]The particle plugging agent (4%) of unaged, aged 10 days and 30 days samples was combined with calcium carbonate particles (8%), fibers (0.2%, 3~5mm, carbon fiber) and elastic graphite (4%), added Add the 4% bentonite base slurry...

Embodiment 3

[0044] Same as Example 1, the difference is: the epoxy monomer (50%) used is E51 and trimethylolpropane triglycidyl ether-TMTGE, and the auxiliary agent is zinc acetylacetonate-Zn(acac) 2 (2%). The heating and curing process is as follows: curing at 90 °C for 2 hours, curing at 120 °C for 1 hour, and curing at 150 °C for 4 hours.

[0045] The glass transition temperature of the solid product obtained in this example is 176°C, and the temperature at which the thermal weight loss is 5% is 300°C; the solid product sample is immersed in oil, aged in an oven at 180°C for 10 days, with a mass loss of 5.5%, and aged for 30 days , with a mass loss of 76%.

[0046] Unaged, aged 10 days, and 30 days samples of particulate loss-stopping agent (4%) were combined with calcium carbonate particles (12%), fibers (0.2%) and elastic graphite (6%), added to a 4% bentonite base slurry In the test slurry, the experimental slurry was formed; a long crack (3×2mm) plugging experimental device was u...

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Abstract

The invention discloses dynamic crosslinking degradable epoxy resin and a preparation method and high-temperature leaking stoppage application thereof. The preparation method of the dynamic crosslinking degradable epoxy resin comprises the following steps that an epoxy monomer, a curing agent and an auxiliary are heated, mixed, heated and cured, a solid product is obtained, the epoxy monomer is a monomer containing 2-4 epoxy groups, the curing agent is anhydride, polyamine and / or a curing agent containing disulfide bonds, and the auxiliary is a solvent. The auxiliary agent is at least one of zinc acetate, acetylacetone, 1, 8-diazabicyclo [5.4. 0] undec-7-ene, diphenyl disulfide, phenol, 2-amino-2-methyl-1-propanol and ethylene glycol amine. According to the invention, the dynamically cross-linked (dynamic sulfur-sulfur bond and dynamic ester exchange bond cross-linked) epoxy resin is prepared to prepare the high-temperature leaking stoppage material capable of being used at 150-210 DEG C, and the obtained material can be gradually degraded at high temperature and lose pressure-bearing leaking stoppage capability, so that the purposes of self-plugging removal and leakage layer protection are achieved.

Description

technical field [0001] The invention relates to a dynamically cross-linked degradable epoxy resin, a preparation method thereof, and a high-temperature plugging application, and belongs to the technical field of drilling intelligent plugging. Background technique [0002] The development of fractures in the reservoir can easily lead to the loss of drilling fluid and cause reservoir damage. Reservoir leakage control requires efficient plugging during drilling and completion, and effective removal of plugging after drilling and completion, so as to restore the seepage capacity of fracture channels in the later stage and meet the needs of reservoir protection. [0003] Commonly used technologies such as bridging and plugging (bridging and plugging cracks with inert particle plugging materials), gel plugging and cement slurry plugging are used to achieve leakage control. To achieve plugging removal, for example, using calcium carbonate particles and other bridging plugging mate...

Claims

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Application Information

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IPC IPC(8): C08G59/42C08G59/22C08G59/38C08G59/50C08G59/58C09K8/467
CPCC08G59/4215C08G59/22C08G59/38C08G59/5006C08G59/502C08G59/504C08G59/5033C08G59/58C08G59/423C09K8/426C09K8/467Y02W30/62
Inventor 范白涛邢希金刘莲英周长所冯桓榰何松王超周定照谷林秦玮
Owner CNOOC TIANJIN BRANCH
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