IP Library › Granted Patent US 12,202,932
Granted Patent B2
US 12,202,932 · App. 17/658,391 · Granted Jan 21, 2025

Formulation and processing of degradable high Tg epoxy composite that can be degradable at extremely low temperature

Inventors: Lei Zhao (Houston, TX); Jiaxiang Ren (Houston, TX); Cheng Peng (Houston, TX); Yu Liu (Beijing, CN)
Assignees: CNPC USA CORPORATION; BEIJING HUAMEI, INC.; CHINA NATIONAL PETROLEUM CORPORATION
C08G59/24C08G59/682C08J3/24C08K5/07C08J2363/00
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Quick Facts
Patent No.
US 12,202,932
App. No.
17/658,391
Granted
Jan 21, 2025
Kind
B2
Abstract

The patent application discloses a degradable thermoset composite. The composite comprises a reaction product of an epoxy resin, a cross-linker, a catalyst. The epoxy resin mixture may comprise at least one cycloaliphatic epoxide. The reaction product may have a glass transition temperature greater than or equal to 140° C. as measured by DMA.

Claims (13)

1. A degradable thermoset composite, comprising a reaction product of:

an epoxy resin, wherein the epoxy resin comprises at least one cycloaliphatic epoxide;

a cross-linker; fibers, wherein fibers are at least one of glass fibers, carbon fibers, aramid fibers, wherein loadings of fibers are from about 20% to about 40% in volume; and

a catalyst for accelerating hydrolysis of the thermoset composite, wherein the catalyst comprises a solid inorganic acid; wherein the cycloaliphatic epoxide comprises bis-(3,4-epoxycyclohexyl) adipate;

wherein the degradable thermoset composite has a glass transition temperature greater than or equal to about 140° C. as measured by DMA, wherein the reaction product has a tensile strength of at least about 10,000 psi, wherein the cross-linker comprises a cycloaliphatic anhydride, the cycloaliphatic anhydride comprises norbornene-based dicarboxylic anhydride, the norbornene-based dicarboxylic anhydride comprises nadic anhydride, wherein the degradable thermoset composite degrades from about 80° C. to about 150° C. under water or brine, wherein stoichiometric ratio between the cycloaliphatic epoxide and the norbornene-based dicarboxylic anhydride is about from about 1:1 to about 1:1.5, wherein ratio between the cycloaliphatic epoxide and the catalyst is about 1:08 to about 1:1.2 by weight.

2. A process for forming a degradable thermoset composition, the process comprising:

admixing an epoxy and a cross-linker to form a mixture at room temperature;

adding a catalyst to the mixture, wherein the catalyst is for accelerating hydrolysis of the thermoset composite, wherein the catalyst comprises a solid inorganic acid; and

mixing with fibers to make raw materials, wherein the epoxy comprises at least one at least one cycloaliphatic epoxide, wherein fibers are at least one of glass fibers, carbon fibers, aramid fibers, wherein loadings of fibers are from about 20% to about 40% in volume; wherein the cycloaliphatic epoxide comprises bis-(3,4-epoxycyclohexyl) adipate;

wherein the degradable thermoset composite has a glass transition temperature greater than or equal to about 140° C. as measured by DMA, wherein the reaction product has a tensile strength of at least about 10,000 psi, wherein the cross-linker comprises a cycloaliphatic anhydride, the cycloaliphatic anhydride comprises norbornene-based dicarboxylic anhydride, the norbornene-based dicarboxylic anhydride comprises nadic anhydride, wherein the degradable thermoset composite degrades from about 80° C. to about 150° C. under water or brine, wherein stoichiometric ratio between the cycloaliphatic epoxide and the norbornene-based dicarboxylic anhydride is about from about 1:1 to about 1:1.5, wherein ratio between the cycloaliphatic epoxide and the catalyst is about 1:08 to about 1:1.2 by weight.

3. The process of claim 2 further comprising molding raw materials into near-net shape parts with hot press.

4. The process of claim 3 further comprising post treating the near-net shape parts.

5. The process of claim 3 , wherein the molding process is conducted within 24 hours without a pre-cure process.

Assignments (1)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Apr 8, 2022
From: ZHAO, LEI; REN, JIAXIANG; PENG, CHENG; LIU, YU
To: CNPC USA CORPORATION; BEIJING HUAMEI INC.; CHINA NATIONAL PETROLEUM CORPORATION
Reel/Frame 059549/0784 →
Continuity (1)
Related Publication 20230323015A1 · Oct 12, 2023
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