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Bio-based hyperbranched polymer epoxy resin and preparation method thereof

A technology of hyperbranched polymer and epoxy resin, applied in the field of high-performance polymer resin, can solve the problems of lack of thermal and mechanical properties, secondary environmental pollution, etc., to improve mechanical properties, low cost of raw materials, reduce Effects of Viscosity and Cure Shrinkage

Pending Publication Date: 2022-04-26
SOUTH CENTRAL UNIVERSITY FOR NATIONALITIES
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It has been reported that epoxy resins containing dynamic covalent bonds usually do not have strong thermal and mechanical properties, so it is necessary to design a high-performance reprocessable epoxy resin
In addition, the current chemical degradation process of epoxy resin requires the use of a large amount of organic solvents, and only part of the degradation products can be reused, which is easy to cause secondary environmental pollution

Method used

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  • Bio-based hyperbranched polymer epoxy resin and preparation method thereof
  • Bio-based hyperbranched polymer epoxy resin and preparation method thereof
  • Bio-based hyperbranched polymer epoxy resin and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Mix 194.0g ferulic acid (FA) and 1295.0g epichlorohydrin (ECH) evenly, stir and react at 80°C for 4h, then add 300.0g 40wt.% sodium hydroxide aqueous solution and continue to react at 30°C for 2h. After the reaction is finished, filter, wash, and separate liquids, dry the organic layer with anhydrous sodium sulfate, and then distill under reduced pressure to remove epichlorohydrin to obtain linear ferulic acid epoxy resin (FEP). The yield is about 86.6%, and the epoxy value It is 0.53mol / 100g.

[0040]300.0g FEP and 43.7g trimethylolpropane were stirred and reacted at 110°C for 6h to obtain ferulic acid hyperbranched epoxy resin FEHBP. The number average molecular weight was 4887g / mol and the epoxy value was 0.29mol / 100g by GPC. .

[0041] 153.6 g of citric acid and 11.2 g of itaconic anhydride were stirred and reacted at 100°C for 6 hours to obtain a citric acid-based hyperbranched epoxy resin CHBP. The number average molecular weight was 1504 g / mol and the acid value...

Embodiment 2

[0049] Mix 194.0g ferulic acid (FA) and 1104.0g epichlorohydrin (ECH) evenly, stir and react at 100°C for 3h, then cool down to room temperature and add 320.0g 30wt.% sodium hydroxide aqueous solution to continue the reaction for 3h. After the reaction is finished, filter and wash with water, dry the organic layer with anhydrous sodium sulfate and distill under reduced pressure to remove epichlorohydrin to obtain linear ferulic acid epoxy resin (FEP), with a yield of about 84.6%, and an epoxy value of 0.52mol / 100g.

[0050] 300.0g FEP and 81.2g trishydroxyethyl isocyanurate were stirred and reacted at 120°C for 4h to obtain a ferulic acid hyperbranched epoxy resin FEHBP. The number average molecular weight was 5458g / mol by GPC test, and the epoxy value was 0.20mol / 100g.

[0051] 499.2g of citric acid and 11.2g of itaconic anhydride were heated and mixed at 120°C for 6 hours to obtain a citric acid-based hyperbranched epoxy resin CHBP. The number average molecular weight was ...

Embodiment 3

[0059] Mix 194.0g ferulic acid (FA) and 1472.0g epichlorohydrin (ECH) evenly, stir and react at 80°C for 4h, then cool down to room temperature and add 600.0g 20wt.% sodium hydroxide aqueous solution to continue the reaction for 4h. After the reaction finishes, filter and wash with water, and the organic layer is dried with anhydrous sodium sulfate to obtain linear ferulic acid epoxy resin (FEP) after decompression distillation and removal of epichlorohydrin, with a yield of 82.1%, and an epoxy value of 0.54mol / 100g.

[0060] 300.0 g of FEP and 30.0 g of glycerol were stirred and reacted at 120°C for 4 hours to obtain a citric acid-based hyperbranched epoxy resin CHBP. The number-average molecular weight was 5799 g / mol and the epoxy value was 0.19 mol / 100 g by GPC.

[0061] 384g of citric acid and 112g of itaconic anhydride were heated and mixed at 120°C for 6 hours to obtain a citric acid-based hyperbranched epoxy resin CHBP. The number average molecular weight was 458g / mol ...

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Abstract

The invention discloses bio-based hyperbranched polymer epoxy resin. The resin is prepared from ferulic acid hyperbranched epoxy resin and citric acid hyperbranched polyester through dynamic crosslinking. The invention also discloses a preparation method of the resin. The epoxy resin prepared by the invention is obtained by dynamically cross-linking ferulic acid hyperbranched epoxy resin and citric acid hyperbranched polyester, a large number of interface covalent bonds are formed in a cross-linked network structure, and the epoxy resin is endowed with a repeatable processing function; under the action of a sodium hydroxide aqueous solution, ferulic acid and citric acid hyperbranched polyester can be controllably degraded, and the degradation products of ferulic acid and citric acid hyperbranched polyester can be used for preparing full-bio-based epoxy resin again, so that green closed-loop recovery of epoxy resin is realized. The resin prepared by the method has excellent mechanical properties, heat resistance, solvent resistance, hydrolysis resistance, creep resistance and corrosion resistance, can replace petroleum-based epoxy resin, and is applied to the fields of electronic packaging, insulating materials, printed circuit boards and the like.

Description

technical field [0001] The invention relates to the technical field of high-performance polymer resins, in particular to a bio-based hyperbranched polymer epoxy resin and a preparation method thereof. Background technique [0002] Epoxy resin has the advantages of high strength, good solvent resistance, water and corrosion resistance, and good insulation, so epoxy resin is widely used. Due to the irreversible crosslinking network of epoxy resin, it is very difficult to degrade and recycle it. Most of them are incinerated or landfilled, which not only wastes resources, but also pollutes the environment. Therefore, it is of great significance to design high-performance green recyclable epoxy resins. [0003] Epoxy resins based on dynamic covalent bonds undergo cross-linking network structure rearrangement under external stimuli, which endows them with self-healing and repeatable processing characteristics, and provides an effective way for the green recycling of epoxy resins ...

Claims

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Application Information

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IPC IPC(8): C08L63/00C08L67/00C08J3/24
CPCC08J3/246C08J2363/00C08J2467/00
Inventor 张俊珩钟柳悦韦芳郝彦鑫海艺凡张道洪
Owner SOUTH CENTRAL UNIVERSITY FOR NATIONALITIES
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