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Phosphorus-containing polyimide material and preparation method thereof

A technology of polyimide and polymer, which is applied in the field of phosphorus-containing polyimide materials and its preparation, can solve problems such as processing and molding difficulties, and limit the development of PI, and achieve simple production conditions, high product purity and high yield , Improve the effect of flame retardant performance

Inactive Publication Date: 2012-12-19
SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Although polyimide has many excellent properties, due to the rigidity of its molecular chain itself and the strong interaction between molecules, the common type of PI neither melts nor dissolves until the decomposition temperature, causing its processing and molding The difficulty greatly limits the development of PI

Method used

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  • Phosphorus-containing polyimide material and preparation method thereof
  • Phosphorus-containing polyimide material and preparation method thereof
  • Phosphorus-containing polyimide material and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Add BPAODOPE (6.725g, 0.01mol) and p-phenylenediamine (1.081g, 0.01mol) into a 250ml four-neck flask equipped with a thermometer, nitrogen gas introduction, electric stirrer, reflux condenser and tail gas absorption device, and then add 100ml N-methylpyrrolidone, stirred at room temperature for 4 hours. Then, under the introduction of nitrogen, the temperature was raised to 170°C to continue the reaction for 5 hours, and after the reaction, continue to pass N 2 Bring to room temperature. Then the solution was poured into 300ml of absolute ethanol to precipitate a precipitate, filtered with suction, washed the filter cake with 200ml of absolute ethanol, and dried under vacuum at 100°C for 6 hours to obtain 6.42g of a brown solid with a yield of 86.2%.

Embodiment 2

[0029] Add BPAODOPE (6.725g, 0.01mol) and m-phenylenediamine (1.189g, 0.011mol) into a 250ml four-neck flask equipped with a thermometer, nitrogen gas introduction, electric stirrer, reflux condenser and tail gas absorption device, and then add 100ml Dimethyl sulfoxide, stirred at room temperature for 4 hours. Then, under the introduction of nitrogen, the temperature was raised to 180°C to continue the reaction for 5 hours, and after the reaction, continue to pass N 2 Bring to room temperature. Then the solution was poured into 300ml of absolute ethanol to precipitate a precipitate, filtered with suction, washed the filter cake with 200ml of absolute ethanol, and dried under vacuum at 100°C for 6 hours to obtain 6.53g of light yellow solid with a yield of 87.7%.

Embodiment 3

[0031] Add BPAODOPE (6.725g, 0.01mol) and m-xylylenediamine (1.362g, 0.01mol) into a 250ml four-neck flask equipped with a thermometer, nitrogen gas introduction, electric stirrer, reflux condenser and tail gas absorption device, and then add 150ml of N,N-dimethylformamide was stirred at room temperature for 4 hours. Then, under the introduction of nitrogen, the temperature was raised to 160°C to continue the reaction for 5 hours, and after the reaction, continue to pass N 2 Bring to room temperature. Then the solution was poured into 400ml of absolute ethanol to precipitate a precipitate, filtered with suction, washed the filter cake with 200ml of absolute ethanol, and dried in vacuum at 100°C for 6 hours to obtain 6.71g of a khaki solid with a yield of 86.8%.

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Abstract

A phosphorus-containing polyimide material and a preparation method thereof relate to a chemical synthetic material and a preparation method thereof; the method comprises the following steps: firstly, dissolving a phosphorus-containing dicarboxylic anhydride monomer (BAODOPE) and a diamine monomer in an organic solvent according to a certain ratio, reacting for 2-8 hours; secondly, heating to 160-200 DEG C with the introduction of inert gas, reacting for 3-10 hours; thirdly, after the reaction, cooling to below 100 DEG C, pouring the reaction solution into a lot of solvents for precipitation, performing suction filtration, washing, and drying of the precipitate to obtain s powdery product which is phosphorus-containing polyimide. The material can not only be used for manufacturing high-performance parts in high-tech fields of aviation, spaceflight, electric appliances, machinery, chemical engineering, microelectronics, and the like, but also be used as a fire retardant to be added into various polymers for the preparation of composite materials so as to improve the flame retardation of the polymers. According to the invention, the process production condition is simple; the product purity and yield are high; and the post-treatment process is simple.

Description

technical field [0001] The invention relates to a chemically synthesized material and a preparation method thereof, in particular to a phosphorus-containing polyimide material and a preparation method thereof. Background technique [0002] Polyimide (PI) is a class of high-performance polymer materials characterized by imide rings. It was synthesized as a high-performance polymer material in 1908, developed as a polymer material in the 1950s, and developed in the 1960s. The 1980s entered a period of vigorous development, and the literature and patents of polyimide surpassed other polymer materials in the same period. In the 1980s and 1990s, polyimide materials entered the electronic information, automobile industry, household appliances and other residential areas. In civil equipment, the application field is further expanded. The proportion of polyimide in US patent, world patent and Japanese patent accounts for 59.9%, 87.7% and 86.8% of the total respectively. Therefore,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/10
Inventor 梁兵曹俊王长松洪晓东宁志高
Owner SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY