Method for preparing naphthyl autocatalytic poly-cyanophenyl resin

A polybenzonitrile resin and naphthyl self-catalysis technology is applied in the field of new high temperature resistant polymer material preparation.

Inactive Publication Date: 2018-06-05
HEBEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this monomer only contains naphthyl ether structure and does not contain active amino groups. It still needs to add a small molecule catalyst during curing, and has the disadvantages of long curing time and high post-curing temperature.

Method used

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  • Method for preparing naphthyl autocatalytic poly-cyanophenyl resin
  • Method for preparing naphthyl autocatalytic poly-cyanophenyl resin
  • Method for preparing naphthyl autocatalytic poly-cyanophenyl resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Synthesis of monomer: Add 10.05g (63.14mmol) 1-amino-7-naphthol, 9.03g (65.35mmol) anhydrous potassium carbonate and 40mL N,N-dimethylformamide in a 250mL three-necked flask as a solvent, and then The mixture was heated up to 60° C., and after 1 hour of reaction, 10.93 g (63.14 mmol) of 4-nitrophthalonitrile was added, and the reaction was continued for 6 hours. Remove the solvent by distillation under reduced pressure, and finally transfer the product from the flask to 500mL deionized water, filter under reduced pressure, and wash the filter cake repeatedly with deionized water until the filtrate is clear and transparent, then put the filter cake in a vacuum drying oven at 60°C Dry under vacuum for 24 hours and set aside.

[0023] Curing: Take about 15g of the above-mentioned monomers and melt them in a 250mL glass reactor at 150°C, and stir continuously to react for 30min to obtain a prepolymer. Grind the prepolymer into powder (100 mesh) and pour it into the prepare...

Embodiment 2

[0030] Synthesis of monomer: Add 12.06g (75.76mmol) 1-amino-5-naphthol, 11.06g (80.00mmol) anhydrous potassium carbonate and 45mL N,N-dimethylformamide in a 250mL three-necked flask as a solvent, and then The mixture was heated up to 60° C., and after 1 hour of reaction, 13.11 g (75.82 mmol) of 4-nitrophthalonitrile was added, and the reaction was continued for 6 hours. Remove the solvent by distillation under reduced pressure, and finally transfer the product from the flask to 500mL deionized water, filter under reduced pressure, and wash the filter cake repeatedly with deionized water until the filtrate is clear and transparent, then put the filter cake in a vacuum drying oven at 60°C Under vacuum drying 24 hours, standby, its structural formula is as follows:

[0031]

[0032] Curing: Take about 15g of the above-mentioned monomers and melt them in a 250mL glass reactor at 210°C, and keep stirring to react for 30min to obtain a prepolymer. Grind the prepolymer into powde...

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Abstract

The invention discloses a method for preparing naphthyl autocatalytic poly-cyanophenyl resin. The method comprises the following steps of (1) adding aminonaphthol, an alkaline catalyst and an organicsolvent in a reactor, performing stirring for 1-2h at the temperature of 60-70 DEG C under the protection of inert atmosphere, then adding 4-nitrophthalonitrile, and performing continuous reaction for6-7h to obtain an autocatalytic cyanophenyl monomer; and (2) putting the autocatalytic cyanophenyl monomer in the reactor, performing melting reaction to obtain a prepolymer, then grinding the prepolymer into powder, transferring the powder into a muffle furnace, rising the temperature from 200-230 DEG C to 280-310 DEG C step by step within 7-9h, and finally obtaining the poly-cyanophenyl resin.By adopting the method provided by the invention, the reaction activity is improved while the melting point of the monomer is lowered, so that the post solidification temperature of the naphthyl autocatalytic poly-cyanophenyl resin is lowered by about 100 DEG C compared with the traditional autocatalytic monomer, the solidification time is reduced by about 8h, and the naphthyl autocatalytic poly-cyanophenyl resin still keeps the characteristics of high temperature resistance and high carbon residue rate.

Description

technical field [0001] The invention belongs to the field of preparation of novel high-temperature-resistant polymer materials, and relates to a preparation method of naphthyl self-catalyzed polybenzonitrile resin. Background technique [0002] Polybenzonitrile resin is a high-performance thermosetting resin formed by the opening and addition polymerization of phthalonitrile monomers through cyano triple bonds. It has been developed by the US Navy Laboratory since the 1970s. Due to its excellent Heat resistance, flame retardancy and chemical stability have been valued by many domestic and foreign scholars. However, since polybenzonitrile monomers and small molecule catalysts need to be cured at high temperatures for a long time, the catalytic efficiency decreases due to the volatilization of the curing agent and defects occur in the resin. In addition, in terms of processing, the problem of melt blending of curing agent and monomer must be solved, which makes the steps comp...

Claims

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Application Information

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IPC IPC(8): C08G73/06
CPCC08G73/065
Inventor 张庆新王建于晓燕
Owner HEBEI UNIV OF TECH
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