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A kind of preparation method of isocyanate-based polyimide rigid foam

An ester-based polyimide and rigid foam technology is applied in the fields of polymer foam materials and high-performance materials. Effect

Active Publication Date: 2020-10-16
BEIJING TECHNOLOGY AND BUSINESS UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are the following defects: different types of catalysts are added at the same time, the chain growth reaction and foaming reaction occur at the same time, and the foam structure is not easy to control

Method used

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  • A kind of preparation method of isocyanate-based polyimide rigid foam
  • A kind of preparation method of isocyanate-based polyimide rigid foam

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Add 100g of pyromellitic anhydride (PMDA) and 25g of methanol into 100g of N,N-dimethylformamide (DMF) and react until clarification at a certain temperature, and then gradually increase the temperature. During the temperature rise to 80°C, add 130g polyphenyl polymethylene polyisocyanate (PAPI), then add 2g stannous octoate catalyst, react at 80-95°C for 3-7 hours to obtain prepolymer solution and cool to room temperature, add 40g PAPI and Stir 2g of triethylamine (TEA) evenly, then add 30g of foam stabilizer AK-8805 and 15g of deionized water, stir at a high speed of 1000-2000r / min for 10-20s and freely foam to obtain a foam intermediate, and finally The foam intermediate is placed in a vacuum drying oven and treated at a high temperature of 160-220°C for 4-6 hours, so that the foam intermediate is fully imidized to obtain a polyimide rigid foam.

Embodiment 2

[0027] Add 100g PMDA and 25g methanol into 100g DMF and react at a certain temperature until clarification, and then gradually increase the temperature. When the temperature rises to 80°C, add 130g PAPI, and then add 2g dibutyltin dilaurate (DBTDL) catalyst, React at 80-95°C for 3-7 hours to obtain a prepolymer solution and cool it down to room temperature, add 40g of PAPI and 2g of triethanolamine (TEOA) and stir evenly, then add 30g of foam stabilizer AK-8805 and 15g of deionized The water is stirred at a high speed of 1000-2000r / min for 10-20s and foamed freely to obtain a foam intermediate, and finally the foam intermediate is placed in a vacuum drying oven at a high temperature of 160-220°C for 4-6 hours, so that The foam intermediate is fully imidized to obtain polyimide rigid foam.

Embodiment 3

[0029] 100g PMDA and 25g methyl alcohol are added in 100g DMF and react to clarification at a certain temperature, then gradually heat up, in the process that temperature rises to 80 ℃, add 130g PAPI, then add catalyst dibutyltin dilaurate (content is 0.74wt %), reacted at 80-95°C for 3-7 hours to obtain a prepolymer solution and cooled to room temperature, then added 40g of PAPI and triethanolamine (0.74wt%) and stirred evenly, then added 30g of foam stabilizer AK- 8805 and 15g of deionized water are stirred at a high speed of 1000-2000r / min for 10-20s and foamed freely to obtain a foam intermediate, and finally the foam intermediate is placed in a vacuum drying oven at 160-220°C for high temperature treatment4 ~6 hours, the foam intermediate is fully imidized, and the scanning electron microscope photo of the polyimide rigid foam is as follows figure 1 shown.

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Abstract

The invention discloses a preparation method of isocyanate based polyimide hard foam which is synthesized by taking aromatic dianhydride and isocyanate as main raw materials. The preparation method ofthe isocyanate based polyimide hard foam mainly comprises the following steps: preparation of prepolymer, a foaming process and a control process on high-temperature after-treatment. Foam materials with different structures and performance are obtained by regulating proportions of organic tin catalysts to amine catalysts. Compared with other polyimide foams, the prepared foam is low in manufacturing cost, is simple in preparation process, is low in equipment requirement, has good mechanical properties, has excellent thermal stability and flame resistance, and has a limited oxygen index beingas high as 49.2%. According to the preparation method disclosed by the invention, deionized water is taken as a foaming agent, polyimide foam is prepared by mechanical stirring and foaming, and harmful gas is not generated in a preparation process, so that the preparation method is suitable for industrial continuous production; and an obtained terminal product is expected to be applied in the aspects of high-temperature-resistant heat-insulating materials, flame-resistant materials and the like on a large scale, and has a wide application prospect and a great commercial value.

Description

technical field [0001] The invention relates to a preparation method of isocyanate-based polyimide rigid foam, which belongs to the field of polymer foam materials and also belongs to the field of high-performance materials. Background technique [0002] Polyimide (PI) foam is one of the materials with the best thermal stability among polymer foams. It has excellent self-flammability and good mechanical properties, and can be used as a structural material. However, its production process is difficult to control, difficult to process and manufacture, and its production cost is high. It is mainly used in high-tech fields such as aerospace and electronics industries, which greatly limits its wide application. The preparation process of isocyanate-based polyimide foam is simple, the equipment requirements are loose, and the manufacturing cost is low, so it has attracted attention in recent years. However, the formation reaction of polyimide is a complex chemical reaction system...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08J9/08C08L79/08C08G73/10
CPCC08G73/1035C08J9/08C08J2203/02C08J2379/08
Inventor 田华峰姚媛媛项爱民
Owner BEIJING TECHNOLOGY AND BUSINESS UNIVERSITY
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