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Preparation method of graphene/polyimide composite adhesive

A composite adhesive and polyimide technology, which is applied in the directions of adhesives, adhesive additives, non-polymer adhesive additives, etc., to expand the application prospects, the preparation process is simple and efficient, and the dispersion and compatibility are improved. Effect

Active Publication Date: 2014-11-26
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

And with graphene modified PI adhesive, there is no report yet

Method used

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  • Preparation method of graphene/polyimide composite adhesive
  • Preparation method of graphene/polyimide composite adhesive
  • Preparation method of graphene/polyimide composite adhesive

Examples

Experimental program
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Effect test

Embodiment 1

[0030] (a) Preparation and surface modification of graphene oxide

[0031] Prepare graphite oxide by the improved Hummers method, take 10mg of graphite oxide, add it to 10ml DMAC or DMF organic solvent, and ultrasonically strip it for 3 hours to obtain a suspension of GO / DMAC; then add an appropriate amount of silane coupling agent diluent, KH-550 is 1% of the mass of graphene oxide was fully stirred in a water bath at 70°C for 1 hour to obtain an undried sticky substance.

[0032] (b) Ultrasonic blending of modified graphene oxide and polyamic acid in ice bath

[0033] Add polyamic acid to the above-mentioned dope, the quality of the modified graphene is 2.5% of the polyamic acid quality, after stirring for 5min, ultrasonically blend in the ice bath for 0.5h to obtain a stable suspension which is graphene / polyamic acid. Precursors for imide composites.

[0034] (c) Vacuum thermal imidization of polyamic acid and in situ thermal reduction of graphene oxide

[0035] In the v...

Embodiment 2

[0037] (a) Preparation and surface modification of graphene oxide

[0038] Prepare graphite oxide by the improved Hummers method, take 10mg graphite oxide, add it to 10ml DMAC or DMF organic solvent, and ultrasonically strip it for 2 hours to obtain a suspension of GO / DMAC; then add an appropriate amount of silane coupling agent diluent, KH-550 is 2% of the mass of graphene oxide, fully stirred in a water bath at 60°C for 2 hours to obtain an undried sticky substance.

[0039] (b) Ultrasonic blending of modified graphene oxide and polyamic acid in ice bath

[0040] Add polyamic acid to the above-mentioned viscous substance, the quality of modified graphene is 2% of the mass of polyamic acid, after stirring for 5 minutes, ultrasonically blend in ice bath for 1 hour to obtain a stable suspension that is graphene / polyamide Precursors for imine composites.

[0041] (c) Vacuum thermal imidization of polyamic acid and in situ thermal reduction of graphene oxide

[0042] In the va...

Embodiment 3

[0044] (a) Preparation and surface modification of graphene oxide

[0045] Graphite oxide was prepared by the improved Hummers method. Take 5mg of graphite oxide, add it to 10ml DMAC or DMF organic solvent, and ultrasonically strip it for 1h to obtain a suspension of GO / DMAC; then add an appropriate amount of silane coupling agent diluent, KH-550 is 3% of the mass of graphene oxide, fully stirred in a water bath at 60°C for 2 hours to obtain an undried sticky substance.

[0046] (b) Ultrasonic blending of modified graphene oxide and polyamic acid in ice bath

[0047] Add polyamic acid to the above-mentioned dope, the quality of modified graphene is 0.5% of polyamic acid quality, after stirring for 10min, ultrasonically blend in ice bath for 1.5h to obtain a stable suspension which is graphene / polyamic acid. Precursors for imide composites.

[0048] (c) Vacuum thermal imidization of polyamic acid and in situ thermal reduction of graphene oxide

[0049] In the vacuum oven, a ...

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Abstract

The invention relates to a preparation method of a graphene / polyimide composite adhesive, which comprises the following steps: adding graphite oxide into an organic solvent, carrying out ultrasonic stripping for 0.5-3 hours to obtain a graphene oxide suspension, adding a silane coupling agent dilute solution into the suspension, and stirring in a 60-80 DEG C water bath for 0.5-1 hour to obtain modified graphene oxide; and adding polyamic acid into the modified graphene oxide, stirring, carrying out ultrasonic blending in an ice bath for 0.5-2 hours to obtain a graphene / polyimide composite material precursor, and curing in a vacuum drying oven at different procedure temperatures. The composite adhesive prepared by the method has the advantages of short period, high speed, high efficiency, simple technique and energy saving, is easy to operate, and can be popularized.

Description

technical field [0001] The invention belongs to the field of preparation of composite adhesives, in particular to a preparation method of graphene / polyimide composite adhesives. Background technique [0002] Since PI came out in the 1960s, as a new type of high temperature resistant adhesive, it has been widely used in many fields, especially in the fields of aircraft manufacturing, aviation and machinery industry. Among many adhesives, polyimide adhesives have excellent properties, which are unmatched by other organic adhesives, and thus become the adhesive with the best comprehensive performance. It can be applied to the bonding of metals (titanium alloy, aluminum alloy, stainless steel) and inorganic non-metals (silicon wafers, glass and abrasives such as emery, silicon nitride and other ceramics) and polymers (bulk materials). In addition to excellent solvent stability, high radiation resistance, self-extinguishing, low smoke generation, non-toxic, PI adhesive also has ...

Claims

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Application Information

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IPC IPC(8): C09J179/08C09J11/04C09C1/46C09C3/12C08G73/10
CPCY02P20/10
Inventor 王海风余小霞吴新宇
Owner DONGHUA UNIV
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