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Cross-linking type polyarylene ether nitrile and preparation method thereof

A polyarylether nitrile, cross-linking technology, applied in the field of cross-linking polyarylether nitrile and its preparation, can solve the harsh conditions of cross-linking reaction, limit the large-scale application of polyarylether nitrile, polyarylether nitrile reinforced Limited problems, to achieve the effect of easy industrialization, good heat resistance, and good heat resistance

Inactive Publication Date: 2016-10-26
UNIV OF ELECTRONICS SCI & TECH OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the small number of crosslinking points, on the one hand, the conditions for the crosslinking reaction to occur are relatively harsh, and on the other hand, the enhancement of polyarylether nitrile by crosslinking is still limited, thus limiting the application of polyarylether nitrile in the field of higher temperature resistance. scale application
Therefore, finding a polyarylether nitrile with a higher crosslinking density is the key to solving the above problems, but there are few patents on the preparation and application of crosslinkable polyarylether nitrile in China at present.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment example 1

[0015] (1) Hydroxy-terminated polyarylether nitriles containing carboxyl groups in the side chain: 0.1mol 2,6-dichlorobenzonitrile, 0.051mol biphenol, and 0.051mol phenolphthalein were added to 75mL of N-methylpyrrolidone, Then add 0.25 mol of potassium carbonate and 25 mL of toluene, dehydrate at 160°C for 2 hours, remove water and part of the toluene, raise the temperature to 200°C and continue the reaction for 3 hours to obtain hydroxyl-terminated polyarylene ether nitrile containing carboxyl groups in the side chain;

[0016] (2) phthalonitrile-terminated polyarylether nitriles containing carboxyl groups in the side chain: the product system obtained in the above step (1) is cooled to 100° C., 0.02mol 4-nitrophthalonitrile is added, and at this temperature React at room temperature for 6 hours, then cool to room temperature, pour the product into acetone, wash and dry to obtain phthalonitrile-terminated polyarylether nitrile with carboxyl group in the side chain;

[0017] ...

Embodiment example 2

[0021] (1) Hydroxyl-terminated polyarylether nitriles containing carboxyl groups in the side chain: 0.1mol 2,6-dichlorobenzonitrile, 0.041mol biphenol, and 0.061mol phenolphthalein were added to 75mL of N-methylpyrrolidone, Then add 0.25 mol of potassium carbonate and 25 mL of toluene, dehydrate at 160°C for 2 hours, remove water and part of the toluene, raise the temperature to 200°C and continue the reaction for 3 hours to obtain hydroxyl-terminated polyarylene ether nitrile containing carboxyl groups in the side chain;

[0022] (2) phthalonitrile-terminated polyarylether nitriles containing carboxyl groups in the side chain: the product system obtained in the above step (1) is cooled to 100° C., 0.02mol 4-nitrophthalonitrile is added, and at this temperature React at room temperature for 6 hours, then cool to room temperature, pour the product into acetone, wash and dry to obtain phthalonitrile-terminated polyarylether nitrile with carboxyl group in the side chain;

[0023]...

Embodiment example 3

[0027] (1) Hydroxy-terminated polyarylether nitriles containing carboxyl groups in the side chain: 0.1mol 2,6-dichlorobenzonitrile, 0.071mol biphenol, and 0.031mol phenolphthalein were added to 75mL of N-methylpyrrolidone, Then add 0.25 mol of potassium carbonate and 25 mL of toluene, dehydrate at 160°C for 2 hours, remove water and part of the toluene, raise the temperature to 200°C and continue the reaction for 3 hours to obtain hydroxyl-terminated polyarylene ether nitrile containing carboxyl groups in the side chain;

[0028] (2) phthalonitrile-terminated polyarylether nitriles containing carboxyl groups in the side chain: the product system obtained in the above step (1) is cooled to 100° C., 0.02mol 4-nitrophthalonitrile is added, and at this temperature React at room temperature for 6 hours, then cool to room temperature, pour the product into acetone, wash and dry to obtain phthalonitrile-terminated polyarylether nitrile with carboxyl group in the side chain;

[0029] ...

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Abstract

The invention relates to cross-linking type polyarylene ether nitrile and a preparation method thereof, belonging to the field of special high-polymer materials. The cross-linking type polyarylene ether nitrile is a polyarylene ether nitrile thermo-solid with a phthalocyanine ring as a crosslinking point. The preparation method for the cross-linking type polyarylene ether nitrile comprises the following steps: preparing polyarylene ether nitrile containing a carboxyl group in its side chain and terminated by a hydroxyl group; then reacting the polyarylene ether nitrile with 4-nitrophthalonitrile so as to obtain nitrophthalonitrile-terminated polyarylene ether nitrile containing the carboxyl group in its side chain; then reacting the polyarylene ether nitrile obtained in the previous step with 3-aminophenoxyl phthalonitrile so as to obtain polyarylene ether nitrile containing phthalonitrile groups in its side chain and terminal; and subjecting the polyarylene ether nitrile obtained in the previous step to processing and molding and then to self-crosslinking at high temperature so as to obtain the cross-linking type polyarylene ether nitrile. The cross-linking type polyarylene ether nitrile has good heat resistance, a glass-transition temperature of 300 DEG C or above and an initial decomposition temperature of 500 to 600 DEG C. The cross-linking type polyarylene ether nitrile is applicable as a high-temperature-resistant structural material and a flame-retardation material to the fields of aviation and spaceflight.

Description

technical field [0001] The invention relates to a cross-linked polyarylether nitrile and a preparation method thereof, belonging to the field of special polymer materials. The bi-type polyarylether nitrile can be used as a high-temperature-resistant structural material and a flame-retardant material in aviation, aerospace and other fields. Background technique [0002] Polyarylene ether nitrile (PEN), as a special thermoplastic resin, has received extensive attention from the commercial and academic circles because of its high temperature resistance, chemical corrosion resistance, radiation resistance, high strength and high modulus, and easy molding and processing. The glass transition temperature (T g ) is not high enough, the modulus drops significantly when applied above the glass transition temperature, and the fluidity has little dependence on temperature at high temperature, thus resulting in a lower use temperature. Cyanoresin is a kind of thermosetting resin, and ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/48C08G65/40C08J5/18C08L71/10
CPCC08G65/48C08G65/4031C08J5/18C08J2371/10C08L71/00C08L2201/02C08L2201/08C08L2203/12C08L2203/16C08L2312/00
Inventor 危仁波童利芬汪佳玲刘孝波
Owner UNIV OF ELECTRONICS SCI & TECH OF CHINA
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