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Reversible self-repairing epoxy resin and preparation method and recovery remodeling method thereof

An epoxy resin, self-healing technology, applied in plastic recycling, recycling technology, organic chemistry, etc., can solve the development trend of low energy consumption and fast recycling and remodeling of packaging resin, can not meet the electronic packaging technology, poor resistance Heat and other problems, to achieve excellent reversible self-healing performance, low remodeling temperature, and the effect of good toughness

Active Publication Date: 2018-08-24
TECHSTORM MATERIAL TECH SHANGHAI CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the lower T g It can guarantee that they can achieve self-healing and recycling remodeling under a certain temperature (R.T.-200°C) and time (0-24h), but their poor heat resistance cannot meet the high-frequency, high-speed, high-density electronic packaging technology. direction development needs
[0007] The existing technology utilizes fragments containing disulfide bonds to prepare reversible self-healing soft materials, but the T g and T di Still low, and their self-healing and remodeling process requires high temperature and long time, which cannot adapt to the development trend of low energy consumption and fast recycling and remodeling of packaging resins

Method used

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  • Reversible self-repairing epoxy resin and preparation method and recovery remodeling method thereof
  • Reversible self-repairing epoxy resin and preparation method and recovery remodeling method thereof
  • Reversible self-repairing epoxy resin and preparation method and recovery remodeling method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0043] 1) Preparation of 2,2'-dithiooxalic acid

[0044] By mass, under the condition that the temperature is 20°C, 120g of 2-mercaptoacetic acid, 500g of ethyl acetate and 0.6g of potassium iodide are uniformly mixed to form solution A; slowly adding 80g of concentration to solution A is after 30wt% hydrogen peroxide, Insulated reaction for 2 hours; after the reaction, the obtained solution was washed with 300 mL of saturated sodium sulfite solution, and ethyl acetate was evaporated under reduced pressure to obtain 2,2'-dithiooxalic acid. For its H NMR spectrum, see the attached figure 1 .

[0045] 2) Preparation of 2,2'-dithiooxalic anhydride

[0046] In terms of mass, at a temperature of 20°C and stirring, 100g of 2,2'-dithiooxalic acid and 150g of trifluoroacetic anhydride were mixed and kept for 2 hours; the resulting solution was evaporated under reduced pressure to remove excess trifluoroacetic anhydride and the resulting After the trifluoroacetic acid of 2,2'-dithioo...

Embodiment 2

[0060] 1) Preparation of 2,2'-dithiooxalic acid

[0061] By mass, at a temperature of 25°C, 120g of 2-mercaptoacetic acid, 600g of methyl acetate and 0.8g of potassium iodide were mixed homogeneously to form a solution A; slowly adding 85g of concentration to the solution A was after 30wt% hydrogen peroxide, Insulated reaction for 3 hours; after the reaction, the obtained solution was washed with 300 mL of saturated sodium sulfite solution, and methyl acetate was evaporated under reduced pressure to obtain 2,2'-dithiooxalic acid.

[0062] 2) Preparation of 2,2'-dithiooxalic anhydride

[0063] In terms of mass, at a temperature of 25°C and under stirring conditions, mix 100g of 2,2'-dithiooxalic acid and 135g of acetic anhydride and keep it warm for 3 hours; 2,2'-Dithiooxalic anhydride is obtained.

[0064] 3) Preparation of reversible self-healing epoxy resin

[0065] In terms of mass, at a temperature of 60°C, glycidyl ester epoxy resin (brand: 672, epoxy equivalent: 161g / ...

Embodiment 3

[0071] 1) Preparation of 2,2'-dithiooxalic acid

[0072] By mass, at a temperature of 30°C, 120g of 2-mercaptoacetic acid, 700g of propyl acetate and 1.0g of potassium iodide were mixed homogeneously to form a solution A; after slowly adding 90g of hydrogen peroxide with a concentration of 30wt% in the solution A, Insulated reaction for 4 hours; after the reaction, the obtained solution was washed with 300 mL saturated sodium sulfite solution, and propyl acetate was evaporated under reduced pressure to obtain 2,2'-dithiooxalic acid.

[0073] 2) Preparation of 2,2'-dithiooxalic anhydride

[0074] In terms of mass, at a temperature of 30°C and under stirring conditions, mix 100g of 2,2'-dithiooxalic acid and 120g of acetic anhydride and keep it warm for 4 hours; 2,2'-Dithiooxalic anhydride is obtained.

[0075] 3) Preparation of reversible self-healing epoxy resin

[0076]By mass, 100g of glycidylamine epoxy resin (brand: AFG-90, epoxy equivalent: 118g / eq), 60g of 2,2'-dithio...

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Abstract

The invention discloses a reversible self-repairing epoxy resin and a preparation method and a recovery remodeling method thereof. Under the catalysis of potassium iodide, an ester solution of 2-thioglycolic acid is oxidized by 30% hydrogen peroxide to obtain 2,2'-dithiooxalic acid. The 2,2'-dithiooxalic acid is subjected to dehydration and cyclization through an anhydride to prepare 2,2'-dithiooxalic anhydride. The 2,2'-dithiooxalic anhydride is mixed with methylhexahydrophthalic anhydride in proportion, an epoxy resin is added, and curing is conducted, so that the reversible self-repairing epoxy resin is obtained. The composition of the dynamic cross-linked network and the permanent cross-linked network in the epoxy resin is changed, the reversible self-repairing and recovery remodelingof the epoxy resin are realized, the excellent heat resistance is obtained, and the mechanical property is improved. The preparation method of the reversible self-repairing epoxy resin provided by theinvention has the advantages of wide raw material source and simple process and the product has the characteristics of being good in applicability and high in practicability.

Description

technical field [0001] The invention relates to a thermosetting resin and a preparation method thereof, in particular to a reversible self-repairing epoxy resin and a preparation, recovery and remodeling method thereof, belonging to the technical field of polymer materials. Background technique [0002] Electronic information is one of the three pillar industries in the 21st century. Big data, intelligent society and sharing economy make electronic information products an indispensable necessity for the entire industrial system and daily life of human beings. Packaging is an important step in the manufacture of electronic products. It mainly undertakes three functions of conduction, insulation and support, which largely determine the performance, quality and manufacturing cost of integrated circuits. Due to its outstanding comprehensive performance, epoxy resin has accounted for more than 90% of the packaging resin used in integrated circuits and semiconductor components. I...

Claims

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Application Information

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IPC IPC(8): C08G59/40C08G59/42C08J11/04C07D327/00C08L63/00
CPCC07D327/00C08G59/4014C08G59/4064C08G59/4238C08J11/04C08J2363/00Y02P20/143Y02W30/62
Inventor 梁国正张又豪顾嫒娟袁莉
Owner TECHSTORM MATERIAL TECH SHANGHAI CO LTD
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