A kind of epoxy resin prepolymer containing hexahydrotriazine structure and preparation method thereof

A technology of epoxy resin and hexahydrotriazine, which is applied in the field of epoxy resin prepolymer containing hexahydrotriazine structure and its preparation, can solve the problems of difficult recycling of composite materials, inability to melt and plasticize, waste of resources, etc. To achieve the effect of controllable and adjustable reaction process, realization of recovery and low viscosity

Active Publication Date: 2020-11-24
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, compared with thermoplastic resins, thermosetting resins generally form prepolymers first, and the potential functional groups in them continue to react to form a crosslinked structure and solidify during molding. This transformation is irreversible. It cannot be melted and plasticized when heated, and it is also insoluble. Composite materials are difficult to recycle
Waste is usually used as filler, landfill or incineration, which not only causes a huge waste of resources, but also brings serious environmental pollution
Therefore, the problem that composite materials are difficult to recycle needs to be solved urgently

Method used

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  • A kind of epoxy resin prepolymer containing hexahydrotriazine structure and preparation method thereof
  • A kind of epoxy resin prepolymer containing hexahydrotriazine structure and preparation method thereof
  • A kind of epoxy resin prepolymer containing hexahydrotriazine structure and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Add 50g of acetaldehyde ammonia trimer and 320g of epichlorohydrin into a 1L three-necked glass flask with a reflux device, then fill the flask with nitrogen, put the three-necked flask into a constant temperature magnetic water bath, and slowly heat up to 90 ℃, continue the reaction for 1 hour after the acetaldehyde ammonia trimer is completely dissolved; after the reaction, cool down to 55 ℃, add 105 g of 50% sodium hydroxide aqueous solution evenly into the three-necked flask within 1 hour, and then continue the reaction for 0.5 hour After completing the ring closure reaction, it was cooled to room temperature. Remove the insoluble matter by filtration, then add 200ml of distilled water to the filtrate, shake well and stand still, then take the lower layer solution. Continuously wash 3 times with distilled water, remove and reclaim unreacted epichlorohydrin at last by rotary evaporation, obtain epoxy resin prepolymer 110g of the present invention, productive rate 95....

Embodiment 2

[0025] Add 50g of acetaldehyde ammonia trimer and 215g of epichlorohydrin into a 1L three-necked glass flask with a reflux device, then fill the flask with nitrogen, put the three-necked flask into a constant temperature magnetic water bath, and slowly heat up to 80 ℃, continue the reaction for 2 hours after the acetaldehyde ammonia trimer is completely dissolved; after the reaction, cool down to 45 ℃, add 130g of 40% sodium hydroxide aqueous solution evenly into the three-necked flask within 1.5 hours, and then continue the reaction for 1 hour After completing the ring closure reaction, it was cooled to room temperature. Remove the insoluble matter by filtration, then add 200ml of distilled water to the filtrate, shake well and stand still, then take the lower layer solution. Continuously wash 3 times with distilled water, remove and reclaim unreacted epichlorohydrin at last by rotary evaporation, obtain epoxy resin prepolymer 101.5g of the present invention, productive rate ...

Embodiment 3

[0027] Add 50g of acetaldehyde ammonia trimer and 120g of epichlorohydrin into a 1L three-necked glass flask with a reflux device, then fill the flask with nitrogen, put the three-necked flask into a constant temperature magnetic water bath, and slowly raise the temperature to 100 ℃, continue the reaction for 0.5h after the acetaldehyde ammonia trimer is completely dissolved; after the reaction, cool down to 50°C, add 85g of 60% sodium hydroxide aqueous solution evenly to the three-necked flask within 1h, and continue the reaction for 1h after the dripping is completed After completing the ring closure reaction, it was cooled to room temperature. Remove the insoluble matter by filtration, then add 200ml of distilled water to the filtrate, shake well and stand still, then take the lower layer solution. Continuously wash 3 times with distilled water, remove and reclaim unreacted epichlorohydrin at last by rotary evaporation, obtain epoxy resin prepolymer 102.8g of the present in...

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Abstract

The invention discloses an epoxy resin prepolymer containing a hexahydrotriazine structure and a preparation method of the epoxy resin prepolymer. The structure of the epoxy resin prepolymer is represented by a formula I. The preparation method is characterized by comprising the following steps: 1) under the protection of inert gas, adding an acetaldehyde ammonia trimer and epoxy chloropropane into a reactor, gradually carrying out heating to 80-100 DEG C under stirring, and after the acetaldehyde ammonia trimer is fully dissolved, continuously carrying out refluxing for 0.5-2h for carrying out a ring-opening reaction; 2) decreasing the temperature to 40-60 DEG C, uniformly and dropwise adding an alkali metal hydroxide solution in 0.5-1.5 hours for carrying out a ring-closing reaction, andcontinuously carrying out the reaction for 0.5-1 hours after the adding is finished; and 3) carrying out purification to obtain a reddish brown viscous liquid product. The epoxy resin prepolymer hassimple preparation process, controllable and adjustable reaction process and high yield, and the prepared composite material can be recycled and is suitable for expanding production.

Description

technical field [0001] The invention relates to the field of epoxy resin, in particular to an epoxy resin prepolymer containing a hexahydrotriazine structure and a preparation method thereof. Background technique [0002] Carbon fiber reinforced epoxy resin-based composites have the characteristics of high specific strength and specific stiffness, good corrosion resistance, and stable structural dimensions. They have been widely used in high-tech fields such as aerospace, wind power, and transportation. However, compared with thermoplastic resins, thermosetting resins generally form prepolymers first, and the potential functional groups in them continue to react to form a cross-linked structure and solidify during molding. This transformation is irreversible. Composites are difficult to recycle. Waste is usually used as filler, landfill or incineration, which not only causes a huge waste of resources, but also brings serious environmental pollution. Therefore, the problem ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D405/14C08G59/50
CPCC07D405/14C08G59/5046
Inventor 袁彦超郑小星赵建青刘述梅
Owner SOUTH CHINA UNIV OF TECH
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