A kind of rosin-based polyamine conductive epoxy curing agent and its preparation method and application

A conductive ring and curing agent technology, used in conductive adhesives, epoxy resin adhesives, adhesives, etc., can solve the problems of high price and high conductive percolation threshold of conductive adhesives, achieve less waste, reduce conductive percolation thresholds, A wide range of effects

Inactive Publication Date: 2018-05-18
INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the conductive percolation threshold of the epoxy resin conductive adhesive can be reduced by these methods, the conductive percolation threshold of the conductive adhesive prepared by these methods is still high, and there are problems such as high price.

Method used

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  • A kind of rosin-based polyamine conductive epoxy curing agent and its preparation method and application
  • A kind of rosin-based polyamine conductive epoxy curing agent and its preparation method and application
  • A kind of rosin-based polyamine conductive epoxy curing agent and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] The purified product of disproportionated rosin, dehydroabietic acid, reacts with tetraethylenepentamine (the molar ratio of dehydroabietic acid to tetraethylenepentamine is 1:4) at 200°C for 3 hours, and removes excess tetraethylene by distillation under reduced pressure. Pentaamine, to obtain a reddish transparent liquid rosin-based polyamine, the structural formula of which is shown in the following formula.

[0029]

[0030] Rosin-based polyamine and graphene are mixed at 1000 rpm (the mass ratio of rosin-based polyamine to graphene is 24:1), and the mixing time is 15min to obtain a black liquid rosin-based polyamine conductive epoxy resin curing agent. Its amine value is 850mgKOH / g, and its conductivity is 4.5S / cm.

[0031] Epoxy resin and rosin-based polyamine conductive epoxy resin curing agent are mixed at a mass ratio of 4:1, and adding 15wt.% silver powder can make the conductivity of epoxy resin reach 4.8×104 S / cm.

Embodiment 2

[0033] The purified product of disproportionated rosin, dehydroabietic acid, was reacted with triethylenetetramine (the molar ratio of dehydroabietic acid to triethylenetetramine was 1:5) at 220°C for 4 hours, and the excess triethylenetetramine was removed by distillation under reduced pressure. Tetramine, the rosin-based polyamine of reddish transparent liquid state is obtained, and its structural formula is as shown in the following formula.

[0034]

[0035] Rosin-based polyamine and carbon nanotubes were mixed at 800 rpm (the mass ratio of rosin-based polyamine to carbon nanotubes was 19:1), and the mixing time was 30 minutes to obtain a black liquid rosin-based polyamine conductive epoxy resin for curing agent, its amine value is 780mgKOH / g, and its conductivity is 4.1S / cm.

[0036] Epoxy resin and rosin-based polyamine conductive epoxy resin curing agent are mixed at a mass ratio of 4:1, and then adding 15wt.% silver powder can make the conductivity of epoxy resin re...

Embodiment 3

[0038] The purified product of disproportionated rosin, dehydroabietic acid, was reacted with diethylenetriamine (the molar ratio of dehydroabietic acid to diethylenetriamine was 1:3) at 200°C for 6 hours, and the excess diethylene was removed by distillation under reduced pressure. triamine, to obtain a reddish transparent liquid rosin-based polyamine, the structural formula of which is shown in the following formula.

[0039]

[0040] Rosin-based polyamine and conductive carbon black were mixed at 1600 rpm (the mass ratio of rosin-based polyamine to conductive carbon black was 3:2), and the mixing time was 30 minutes to obtain a black liquid rosin-based polyamine conductive epoxy resin for curing agent, its amine value is 660mgKOH / g, and its conductivity is 3.4S / cm.

[0041] Epoxy resin and rosin-based polyamine conductive epoxy resin curing agent are mixed in a mass ratio of 4:1, and then adding 35wt.% silver powder can make the conductivity of epoxy resin reach 3.2×10 ...

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Abstract

The invention discloses a rosin-based polyamine conductive epoxy hardener and a preparation method and application thereof. The preparation method includes: enabling dehydroabietic acid which is a disproportionated rosin purification product to react with polyamine, and depressurizing for distilling to remove redundant polyamine to obtain slightly-red transparent liquid rosin-based polyamine; mixing the rosin-based polyamine with a carbonaceous conductive filler to obtain the rosin-based polyamine conductive epoxy hardener. Pi-Pi interaction between rosin-based polyamine and carbonaceous conductive particles like grapheme is utilized creatively to uniformly disperse the carbonaceous conductive particles in rosin-based polyamine, so that sedimentation is avoided; the rosin-based polyamine conductive epoxy hardener prepared by the method has extremely high amine value and conductivity, and can substantially lower percolation threshold value of conductive adhesives when being applied in preparing epoxy resin conductive adhesives.

Description

technical field [0001] The invention relates to the field of epoxy resin curing agent and epoxy resin conductive adhesive, in particular to a rosin-based polyamine conductive epoxy curing agent and its preparation method and application. Background technique [0002] With the gradual development of electronic products towards miniaturization, portability, high sensitivity, and high reliability, the traditional Pb / Sn solder can no longer meet the development requirements due to problems such as material deformation, internal stress, and serious environmental pollution caused by high-temperature welding. . Epoxy resin conductive adhesive has the advantages of high resolution, good environmental performance, simple processing procedure, and is suitable for large-scale production. It can meet the development requirements of electronic products and meet the requirements of sustainable development. It is an ideal substitute for high-pollution Pb / Sn solder. It has been widely used...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G59/50C08K3/04C08K3/08C09J163/00C09J9/02C08L63/00C09F1/04
CPCC08G59/50C08K3/04C08K3/08C08K2003/0806C08L63/00C09F1/04C09J9/02C09J163/00
Inventor 黄金瑞聂小安董建
Owner INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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