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Polyimide adhesive and preparation method thereof

A technology of polyimide adhesives and adhesives, which is applied in the direction of adhesives, etc., can solve the problems of decreased adhesive performance, heat-resistant instability of polyimide adhesives, etc., to achieve glass transition temperature increase, lower melting The effect of improving the bulk viscosity and improving the adhesive performance

Active Publication Date: 2018-10-12
INST OF CHEM CHINESE ACAD OF SCI +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] In view of the above analysis, the present invention aims to provide a polyimide adhesive and a preparation method thereof to solve the problem of thermal instability of the polyimide adhesive and decreased bonding performance when the temperature is higher than 350°C. question

Method used

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  • Polyimide adhesive and preparation method thereof
  • Polyimide adhesive and preparation method thereof

Examples

Experimental program
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Embodiment 1

[0059] (1) In a three-necked flask equipped with a mechanical stirrer, water separator, nitrogen inlet and outlet, and a thermometer, add 28.82 grams (0.09 moles) of 4,4'-diamino-2,2'-bistrifluoromethylbiphenyl, 3.49 g (0.01 mol) of bis(4-aminophenoxy)tetramethyldisiloxane and 110 g of N-methylpyrrolidone were stirred under nitrogen protection until completely dissolved. After that, 16.11 g (0.05 mol) of 3,3',4,4'-benzophenone tetraacid dianhydride and 24.82 g (0.10 mol) of 4-phenylethynylphthalic anhydride were added, and stirred under a nitrogen atmosphere until completely dissolved. Stir at room temperature for 12 hours to obtain a homogeneous solution with a solid content of 40 wt.%.

[0060] (2) Add 16 grams of toluene to the above homogeneous solution, raise the temperature of the reaction system to 175° C., react for 12 hours under nitrogen protection, then raise the temperature to 200° C. to evaporate the toluene and stop heating.

[0061] (3) Cool the reaction soluti...

Embodiment 2

[0066] (1) In a three-necked flask equipped with a mechanical stirrer, water separator, nitrogen inlet and outlet, and a thermometer, add 25.62 grams (0.08 moles) of 4,4'-diamino-2,2'-bistrifluoromethylbiphenyl, 6.97 g (0.02 mol) of bis(4-aminophenoxy)tetramethyldisiloxane and 215 g of N,N-dimethylacetamide were stirred under nitrogen protection until completely dissolved. After that, 19.33 g (0.06 mol) of 3,3',4,4'-benzophenone tetraacid dianhydride and 19.86 g (0.08 mol) of 4-phenylethynylphthalic anhydride were added, and stirred under a nitrogen atmosphere until completely dissolved. Stir at room temperature for 12 hours to obtain a homogeneous solution with a solid content of 25 wt.%.

[0067] (2) 11 grams of xylene was added to the above homogeneous solution, the temperature of the reaction system was raised to 150° C., and the reaction was carried out under nitrogen protection for 12 hours, and then the temperature was raised to 166° C. to evaporate the xylene and stop ...

Embodiment 3

[0073] (1) In a three-neck flask equipped with a mechanical stirrer, a water separator, a nitrogen inlet and outlet, and a thermometer, add 22.42 grams (0.07 moles) of 4,4'-diamino-2,2'-bistrifluoromethylbiphenyl, 10.46 g (0.03 mol) of bis(4-aminophenoxy)tetramethyldisiloxane and 165 g of N,N-dimethylformamide were stirred under nitrogen protection until completely dissolved. After that, 21.49 g (0.067 mol) of 3,3',4,4'-benzophenone tetraacid dianhydride and 16.56 g (0.067 mol) of 4-phenylethynylphthalic anhydride were added, and stirred under a nitrogen atmosphere until completely dissolved. Stir at room temperature for 8 hours to obtain a homogeneous solution with a solid content of 30 wt.%.

[0074] (2) 8 grams of toluene was added to the above homogeneous solution, the temperature of the reaction system was raised to 140° C., and the reaction was carried out under nitrogen protection for 12 hours, and then the temperature was raised to 153° C. to evaporate the toluene and ...

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Abstract

The invention relates to a polyimide adhesive and a preparation method thereof and belongs to the technical field of adhesives. The polyimide adhesive solves the problem that the polyimide adhesive ata temperature of greater than 350 DEG C has poor thermal instability and low adhesive properties. The polyimide adhesive is prepared from a polyimide adhesive prepolymer through curing. The preparation raw materials of the polyimide adhesive prepolymer comprise aromatic diamine containing a biphenyl structure, aromatic diamine containing a siloxane structure, aromatic dianhydride and a blocking agent. The preparation method comprises dissolving the polyimide adhesive prepolymer in an organic solvent to obtain a homogeneous solution, coating the surface of the adherend with the homogeneous solution, removing the organic solvent, carrying out curing to obtain the polyimide adhesive and bonding the adherend The polyimide adhesive can be used for the bonding of high temperature resistant parts in the fields of aviation, aerospace, precision machinery and petrochemical industry.

Description

technical field [0001] The invention relates to the technical field of adhesives, in particular to a polyimide adhesive and a preparation method thereof. Background technique [0002] With the rapid development of aerospace technology, organic heat-resistant adhesives have been widely used in various aircraft manufacturing. [0003] Polyimide adhesives are more and more popular because of their excellent heat resistance and high temperature bonding properties. Generally, polyimide adhesives are classified according to processing and synthesis methods: condensation type, thermoplastic type and addition type. For condensation-type polyimide adhesives, the curing process is the dehydration and cyclization process of polyamic acid, and the formation of water in the middle is easy to form pore defects, which is not suitable for large-scale bonding. For thermoplastic polyimide adhesives, although the material can be bonded by direct hot melting to avoid the generation of pores, ...

Claims

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Application Information

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IPC IPC(8): C09J179/08C08G73/10
CPCC08G73/1007C08G73/1039C08G73/106C08G73/1067C09J179/08
Inventor 范琳刘仪翟磊
Owner INST OF CHEM CHINESE ACAD OF SCI
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