Preparation method of fluorine-containing autocatalytic phthalonitrile resin

A technology of phthalonitrile and nitrophthalonitrile is applied in the field of high temperature resistant polymer material preparation to achieve the effects of avoiding resin defects, novel structure and expanding application scope

Active Publication Date: 2020-07-10
HEBEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are still some gaps in the dielectric properties of traditional polybenzonitrile resins to meet the application of electronic packaging

Method used

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  • Preparation method of fluorine-containing autocatalytic phthalonitrile resin
  • Preparation method of fluorine-containing autocatalytic phthalonitrile resin
  • Preparation method of fluorine-containing autocatalytic phthalonitrile resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Monomer synthesis:

[0029] Add 5.02g (39.49mmol) of 4-amino-3-fluoro-phenol and 8.19g (59.24mmol) of anhydrous potassium carbonate to the reactor, then add 60mL of DMF, heat to 60°C, stir magnetically for 1 hour, add 6.84g (39.49 mmol) 4-nitrophthalonitrile, heated to 80° C. and stirred for 8 hours; after the reaction was stopped, the reaction was distilled under reduced pressure for 0.5 hour to remove most of the DMF solvent. After the final reaction, cool to room temperature, slowly pour the reactant into 0.1mol / L NaOH aqueous solution (700ml), stir evenly until the product precipitates, let stand for 5 hours, filter under reduced pressure, and then wash with a large amount of deionized water until the filtrate It was clear and transparent, and dried under vacuum at 60°C for 24 hours to obtain 4-(4-amino-3-fluoro-phenol)-benzonitrile monomer in the form of reddish-brown solid powder with a yield of 89%.

[0030] The structure is as follows:

[0031]

[0032] Pol...

Embodiment 2～5

[0039] The 4-amino-3-fluoro-phenol in the monomer synthesis step in Example 1 is respectively prepared from 2-amino-5-fluoro-phenol, 3-amino-4-fluoro-phenol, 3-amino-5-fluoro -phenol or 4-amino-2-fluoro-phenol instead, other steps are the same as in Example 1. The structural formula of the obtained fluorine-containing self-catalyzed benzonitrile monomer is as follows:

[0040]

[0041] The performance data of the obtained autocatalytic polyphthalonitrile resin is close to that of Example 1.

Embodiment 6

[0043] Change the amount of potassium carbonate in Example 1 to 51.34 mmol (fluorine-containing aminophenol: basic catalyst=1:1.3), and other steps are the same as in Example 1.

[0044] The chemical reagents are all commercially available.

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Abstract

The invention relates to a preparation method of fluorine-containing autocatalytic phthalonitrile resin. The method comprises the following steps: (1) adding fluorine-containing aminophenol, a basic catalyst, an organic solvent and 4-nitrophthalonitrile into a reactor, and reacting to obtain a fluorine-containing autocatalytic phthalonitrile monomer; and (2) putting the fluorine-containing self-catalyzed cyanophenyl monomer into an aluminum foil mold, and carrying out gradient temperature rise and curing to obtain the fluorine-containing phthalonitrile resin material. The synthesis period is short, the yield is high, the processing technology is simple, and the obtained resin can be widely applied to the fields of composite materials, aerospace, electronic packaging and the like.

Description

technical field [0001] The invention belongs to the field of high-temperature-resistant polymer material preparation, and relates to a fluorine-containing self-catalyzed phthalonitrile resin and a preparation method. Background technique [0002] Phthalonitrile resin (abbreviation: polybenzonitrile resin) is a high temperature resistant material originally developed by the US Naval Research Laboratory. Polybenzonitrile resin is widely used in composite materials, adhesives, There are potential applications in aerospace, electronic packaging and other fields. [0003] Studies have shown that the polymerization reaction of pure phthalonitrile monomers is very slow, requiring long-term heat treatment at high temperatures for the curing reaction to occur. Accelerated phthalonitrile monomer curing agents include: organic amines, phenols, strong organic acids, strong organic acids / amine salts, metal salts, metals, etc. The addition of a small molecule curing agent can effective...

Claims

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Application Information

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IPC IPC(8): C08G73/06C07C253/30C07C255/54
CPCC08G73/0672C07C253/30C07C255/54
Inventor 武敏杰李媛媛张庆新于晓燕
Owner HEBEI UNIV OF TECH
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