Preparation method of rigid polyimide foam material

A technology of polyimide and foam materials, applied in the field of polymer material preparation, can solve the problems of difficult to achieve large-scale preparation, poor adhesion between microspheres, and reduced thermal oxidation resistance, etc., and achieves easy popularization. , The effect of high closed cell rate and cost reduction

Active Publication Date: 2019-07-19
AEROSPACE RES INST OF MATERIAL & PROCESSING TECH +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Rigid polyimide foams that have been commercialized are based on 3,3',4,4'-benzophenone tetra-acid dianhydride (BTDA) and 4,4'-diaminodiphenyl ether (4,4 '-ODA) made of serialized foam products (TEEK-LL), based on 3,3',4,4'-diphenyl ether tetra-acid dianhydride (ODPA) and 4,4'-ODA made of serialized Foam products (TEEK-HH) and TEEK-CL series products based on BTDA and diaminodiphenyl sulfone (DDS). These foam materials are molded by compression molding, and often have poor bonding performance between microspheres. As a result, the compressive strength of the foam is low, and the closed cell rate is not high
[0006] Chinese patent CN102964834A discloses a new method for preparing rigid foam, which uses norbornene anhydride as an end-capping agent to prepare a polyimide resin with a norbornene structure in the main chain, and then utilizes it in the curing and crosslinking process In this system, the released gas expands and foams. The non-aromatic ring conjugated structure is introduced into the system, which reduces the thermal oxidation resistance of the foam when it is used at high temperature for a long time. At the same time, the raw materials prepared by this method are mostly isomers. Mainly biphenyl dianhydride, the cost is extremely high, and it is difficult to realize large-scale preparation on a large scale

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] A preparation method of rigid polyimide foam material, the method may further comprise the steps:

[0031] a. Add 31 g of dried 3,3',4,4'-diphenyl ether tetra-acid dianhydride into a mixed solvent containing 60 g of tetrahydrofuran and 12.8 g of methanol, raise the temperature to 60°C, keep stirring for 3 hours, then cool down to room temperature, Add 41g of 2,2-bis[4-(4-aminophenoxy)phenyl]propane (BAPP), heat up to 60°C and mix for 2 hours, then add 3.6g of AK8805, and discharge to obtain a precursor solution;

[0032] b. Treat the precursor solution in an oven at 90°C for 1 hour, then pulverize it and place it in an oven at 120°C for foaming for 60 minutes;

[0033] c. Hot press the foam obtained above, the hot pressing temperature is 130°C, and the compressive strength is 10MPa, then the sample is placed in a mold at 320°C, the mold is closed and foamed, and the foaming time is maintained for 2 hours, and then the temperature is naturally cooled to room temperature,...

Embodiment 2

[0037] A preparation method of rigid polyimide foam material, the method may further comprise the steps:

[0038] a. Add 31 g of dried 3,3',4,4'-diphenyl ether tetra-acid dianhydride into a mixed solvent containing 60 g of tetrahydrofuran and 12.8 g of methanol, raise the temperature to 60°C, keep stirring for 3 hours, then cool down to room temperature, Add 41g of 2,2-bis[4-(4-aminophenoxy)phenyl]propane (BAPP), heat up to 60°C and mix for 2 hours, then add 3.6g of AK8805 and 3.6g of foaming aid, and discharge to obtain a precursor solution ;

[0039] b. Treat the precursor solution in an oven at 85°C for 1 hour, then pulverize it and place it in an oven at 120°C for foaming for 60 minutes;

[0040] c. Hot press the foam obtained above, the hot pressing temperature is 130°C, and the compressive strength is 10MPa, then the sample is placed in a mold at 320°C, the mold is closed and foamed, and the foaming time is maintained for 2 hours, and then the temperature is naturally coo...

Embodiment 3

[0043] A preparation method of rigid polyimide foam material, the method may further comprise the steps:

[0044] a. Add 32.2g of dried 3,3',4,4'-diphenyl ether tetra-acid dianhydride into a mixed solvent containing 50g of tetrahydrofuran and 12.8g of methanol, raise the temperature to 60°C, keep stirring for 3h and then cool down to room temperature , add 29.2g 1,3-bis(4'-aminophenoxy)benzene (1,3,4-APB), heat up to 60°C and mix for 2 hours, then add 3.6g AK8805, 7.0g foaming aid, and discharge Obtain precursor solution;

[0045] b. Treat the precursor solution in an oven at 90°C for 1 hour, then pulverize it and place it in an oven at 100°C for foaming for 30 minutes;

[0046] c. Hot press the foam obtained above, the hot pressing temperature is 110°C, and the compressive strength is 10MPa, then the sample is placed in a mold at 300°C, the mold is closed and foamed, and the foaming time is maintained for 2 hours, and then the temperature is naturally cooled to room temperat...

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Abstract

The invention relates to a hard polyimide foam material and a preparation method thereof, and belongs to the technical field of preparation of high-molecular polyimide foam materials. The preparationmethod comprises the steps of adding an aromatic dianhydride into a tetrahydrofuran/fatty alcohol mixed solvent, and conducting heating to dissolve the aromatic dianhydride; after the solution is transparent, adding an aromatic diamine for reaction to form a foam precursor solution, then adding a foam stabilizer and a foaming aid, and conducting uniform mixing; placing the solution in a drying oven to remove the solvent, and then raising the temperature to carry out primary foaming; and carrying out mold pressing on a primary foamed product to a compact state, further raising the temperature,and carrying out secondary foaming to obtain the polyimide foam. The method has the characteristics of low preparation cost, rich candidate raw materials, easiness in realizing large-scale productionand the like; and the prepared foam material has the characteristics of being uniform in foam structure, adjustable in apparent density, high in compressive strength, high in closed cell rate and almost free of slag falling.

Description

technical field [0001] The invention relates to a rigid polyimide foam material and a preparation method thereof, which belong to the technical field of polymer material preparation. The rigid foam refers to no flexibility, high compressive strength, and deformation after the stress reaches a certain value. , A foam material that cannot return to its original shape after stress relief. Background technique [0002] Polyimide foam material is a high-performance foam material with good mechanical properties, excellent flame retardant properties, and fire resistance. Compared with other types of foam plastics, it does not produce harmful gases during use and has a low density. , a wide range of performance adjustment, easy to install and disassemble, high temperature resistance, but also has excellent low temperature brittleness and other characteristics, has been widely used as heat insulation and noise reduction materials abroad. [0003] Rigid polyimide foam is a kind of po...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/10C08J9/04C08L79/08
CPCC08G73/1071C08J9/04C08J2379/08
Inventor 马晶晶酒永斌赵一搏滕冲熊春晓许小强马晓静
Owner AEROSPACE RES INST OF MATERIAL & PROCESSING TECH
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