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Degradable epoxy resin and preparation method thereof

A technology of epoxy resin and spiral ring structure, which is applied in the field of acid-degradable epoxy resin and its preparation, can solve the problems of environmental pollution, large annual consumption, waste of petroleum resources, etc., and achieve high reactivity and adjustable degradation speed , the effect of fast degradation rate

Active Publication Date: 2019-12-17
TECHSTORM MATERIAL TECH SHANGHAI CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] As we all know, epoxy resin has a wide range of uses and a huge annual consumption, but the chemical properties of epoxy resin after cross-linking and curing are very stable, and it is difficult to degrade it by physical or chemical methods
Discarded epoxy resin curing materials cannot be reused, and usually can only be buried or incinerated, which not only pollutes the environment, but also causes a waste of petroleum resources

Method used

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  • Degradable epoxy resin and preparation method thereof
  • Degradable epoxy resin and preparation method thereof
  • Degradable epoxy resin and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] A kind of synthetic method of degradable epoxy resin, comprises the following steps:

[0045] S1: Add 0.5872g (2.77mmol) BTU, 0.3914g (4.16mmol) ethanedithiol and 35.5mg (0.139mmol) benzoin dimethyl ether into the flask, dissolve it with 2.946g tetrahydrofuran, and put it under the ultraviolet lamp (the light intensity is 3000μW / cm 2 ) under irradiation for 3h. Then the product was precipitated with 20 g of ether, and after centrifugation, the obtained product was put into a vacuum drying oven and dried to constant weight.

[0046] S2: Under a nitrogen atmosphere, 0.5748 g (0.22 mmol) of the product of step S1, 1.506 g (13.2 mmol) of allyl glycidyl ether (AGE) and 2.935 g of chloroform were placed in a round bottom flask. Then under ultraviolet light (light intensity is 3000μW / cm 2) under reaction for 3h. Precipitate three times in 20 g of ether, obtain the product after centrifugation, put it into a vacuum drying oven and dry to constant weight to obtain a degradab...

Embodiment 2

[0051] A kind of synthetic method of degradable epoxy resin, comprises the following steps:

[0052] S1: Add 0.5869g (2.77mmol) of BTU, 1.304g (13.85mmol) of ethanedithiol and 4.7mg (0.028mmol) of azobisisobutyronitrile into the flask, and dissolve them with 11.741g of 1,4-dioxane Dissolved and reacted at 80°C for 6h. The product was precipitated with 30 g of ether, and after centrifugation, the product was placed in a vacuum drying oven to constant weight.

[0053] S2: Under a nitrogen atmosphere, 0.6527g (0.39mmol) of the product of step S1, 90mg (0.78mmol) of AGE and 2.957g of chloroform were placed in a round bottom furnace. Then under ultraviolet light (light intensity is 9000μW / cm 2 ) under reaction for 1h. Precipitate three times in 20 g of ether, obtain the product after centrifugation, put it into a vacuum drying oven and dry to constant weight to obtain a degradable epoxy resin.

[0054] The structure of embodiment 2 product has been characterized with infrared s...

Embodiment 3

[0058] A kind of synthetic method of degradable epoxy resin, comprises the following steps:

[0059] S1: Add 0.5303g (2.50mmol) BTU, 0.5437g (5.0mmol) 1,3-propanedithiol and 13mg (0.05mmol) azobisisoheptanonitrile into the flask, and use 5.31g N,N-dimethyl It was dissolved in formamide and reacted at 60°C for 24h. The product was precipitated with 64 g of diethyl ether, and after centrifugation, the product was put into a vacuum drying oven to constant weight.

[0060] S2: Under an argon atmosphere, 0.4185 g (0.20 mmol) of the product of step S1, 0.228 g (2.0 mmol) of AGE and 3.073 g of chloroform were placed in a round bottom flask. Then under ultraviolet light (light intensity is 6000μW / cm 2 ) under reaction for 2.5h. Precipitate three times in 57g ether, obtain the product after centrifugation, put it into a vacuum drying oven and dry to constant weight to obtain a degradable epoxy resin.

[0061] The structure of embodiment 3 product uses 1 Characterized by H NMR, the...

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Abstract

The invention belongs to the field of new materials, and particularly discloses a degradable epoxy resin and a preparation method thereof. The method is characterized in that a sulfydryl-terminated intermediate compound containing a spiro structure and the epoxy resin containing the spiro structure are synthesized through double sulfydryl-alkene addition reactions, and the molecular weight of theepoxy resin is about 600-5000 g / mol. The cured epoxy resin containing the spiro structure can be completely degraded within 36 h under an acidic condition at a temperature of above 40 DEG C. The method has the advantages of simple process, and rapidness in reaction, and the product has a high reaction activity, can be completely degraded, and is expected to be applied to the fields of epoxy resin-toughened and carbon fiber-reinforced composite materials.

Description

technical field [0001] The invention relates to an acid-degradable epoxy resin containing a spiro ring structure and a preparation method thereof, belonging to the technical field of new polymer materials. Background technique [0002] Traditional epoxy resins (such as bisphenol-A epoxy resins) contain rigid benzene rings and flexible ether bonds in the molecular backbone, so their chemical properties are very stable. Epoxy resin cured with multi-component organic amine or acid anhydride has a three-dimensional cross-linked network structure and has excellent mechanical properties, corrosion resistance and adhesion to polar substrates. At present, it has been widely used in many fields such as anti-corrosion coatings, high-performance adhesives and carbon fiber / glass fiber reinforced composite materials. [0003] As we all know, epoxy resin has a wide range of uses and a huge annual consumption, but the chemical properties of epoxy resin after cross-linking and curing are v...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G59/30C08G59/50
CPCC08G59/302C08G59/5026
Inventor 郑耀臣赵世坤宋鹏班庆福高正国张新涛
Owner TECHSTORM MATERIAL TECH SHANGHAI CO LTD
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