A kind of preparation method of polycondensation type graphene/polyimide composite adhesive

A composite adhesive and graphene technology, applied in the direction of adhesives, adhesive additives, non-polymer adhesive additives, etc., can solve problems such as uneven dispersion, achieve uniform composition, expand application prospects, and improve solubility and dispersion.

Active Publication Date: 2019-05-07
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The composite adhesive prepared by in-situ polymerization effectively avoids the problem of uneven dispersion of graphene nanoparticles mechanically mixed into the polymer matrix

Method used

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  • A kind of preparation method of polycondensation type graphene/polyimide composite adhesive
  • A kind of preparation method of polycondensation type graphene/polyimide composite adhesive
  • A kind of preparation method of polycondensation type graphene/polyimide composite adhesive

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] (1) Oxidation of graphite powder:

[0043] 85ml of concentrated H with a mass fraction of 98% 2 SO 4 solution and 15ml mass fraction of 80% concentrated H 3 PO 4 The solution was successively added into a round-bottomed flask with a volume of 250ml, mechanically stirred and mixed with a stirrer at a speed of 300rpm for 5min, and 1g of graphite powder (flake graphite, particle size≤30μm, proportion≥95%) was added to the resulting mixed acid solution , continue to stir at a speed of 300rpm until the system is evenly mixed, and 5g KMnO 4 Slowly add a small amount to the above solution several times, and stir for 30 minutes at a rotation speed of 350 rpm; under the condition of oil bath temperature control, stir and react at 40°C for 2h, then raise the temperature to 90°C and stir for 1.5h. Subsequently, the excess KMnO was reduced by adding a dilute hydrogen peroxide solution with a mass fraction of 4.5% 4 , Obtain graphite oxide mixed solution; The preparation method...

Embodiment 2

[0056] (1) Oxidation of graphite powder:

[0057] 90ml of concentrated H with a mass fraction of 98% 2 SO 4 solution and 10ml mass fraction is 81% concentrated H 3 PO 4 The solution was successively added into a round bottom flask with a volume of 250ml, mechanically stirred and mixed with a stirrer at a speed of 310rpm for 5min, and 1g of graphite powder (flake graphite, particle size≤30μm, proportion≥95%) was added to the resulting mixed acid solution , continue to stir at a speed of 300rpm until the system is evenly mixed, and 6g KMnO 4 Slowly add small amounts to the above solution several times, and stir at 350 rpm for 25 minutes; under oil bath temperature control, stir and react at 40°C for 2h, then raise the temperature to 90°C and stir for 1.5h. Subsequently, the excess KMnO was reduced by adding a dilute hydrogen peroxide solution with a mass fraction of 4.5% 4 , Obtain graphite oxide mixed solution; The preparation method of described hydrogen peroxide is that ...

Embodiment 3

[0069] (1) Oxidation of graphite powder:

[0070] 91ml of concentrated H with a mass fraction of 98% 2 SO 4 solution and 9ml mass fraction of 82% concentrated H 3 PO 4 The solution is successively added into a round bottom flask with a volume of 250ml, mechanically stirred and mixed for 5min at 310rpm with a stirrer, and 1.5g of graphite powder (flaky graphite, particle size≤30 μm, accounting for≥95% ), continue to stir at 300rpm until the system is evenly mixed, and 7g KMnO 4 Slowly add small amounts to the above solution several times, and stir at 350 rpm for 25 minutes; under oil bath temperature control, stir and react at 40°C for 2h, then raise the temperature to 90°C and stir for 1.5h. Subsequently, the excess KMnO was reduced by dropping a 3% dilute hydrogen peroxide solution 4 , Obtain graphite oxide mixed solution; The preparation method of described hydrogen peroxide is: in the beaker that fills 100ml deionized water, add 10ml mass fraction and be 30% H 2 o 2 ...

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Abstract

The invention relates to a preparation method of a polycondensation type graphene / polyimide composite adhesive. The preparation method comprises the following steps: carrying out ultrasonic dispersion on an amino functionally modified graphene oxide FGO solution, then respectively adding a diamine monomer 4,4'-diaminodiphenyl ether ODA and 2,2-bis[4-(4-aminophenoxy)phenyl]propane BAPP at 2-5DEG C, adding a solvent N-methyl pyrrolidone NMP, stirring for 30-40 minutes at constant temperature in nitrogen protective atmosphere, then adding 3,3',4,4'-benzophenonetetracarboxylic dianhydride BDTA, and continuously stirring for 8-10 hours at the constant temperature, thus obtaining the polycondensation type graphene / polyimide composite adhesive. The preparation method provided by the invention has the advantages that raw materials are available, price is low, no environmental pollution is produced, and green chemistry requirement is met, so that the preparation method can be popularized and applied.

Description

technical field [0001] The invention belongs to the field of preparation of composite adhesives, in particular to a preparation method of polycondensation type graphene / polyimide composite adhesives. Background technique [0002] Since the commercialized polyimide (PI) material was introduced, PI has been widely applied and researched, especially in the research of high temperature resistant polymer materials, which has strong practical application research significance. PI adhesive has excellent solvent stability, heat resistance, high radiation resistance, thermal oxidation resistance, chemical corrosion resistance, low smoke rate, non-toxic and excellent mechanical properties, which are beyond the reach of other organic adhesives Compared with it, it becomes the high temperature resistant adhesive with the best comprehensive performance. It can be applied to bonding metals (such as copper, aluminum, titanium alloys, aluminum alloys and stainless steel, etc.), inorganic n...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G73/10C09J179/08C09J11/04
CPCC08G73/1071C08K3/04C08K9/04C09J11/04C09J179/08
Inventor 王海风张亚飞庆健
Owner DONGHUA UNIV
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