Double end-group phthalonitrile, resin, condensate and its preparation method and uses

A technology of phthalonitrile resin and base phthalonitrile, which is applied in the field of polymer synthetic materials, can solve the problems of poor performance of cured products, complicated reaction mechanism, large creep at high temperature and the like, and achieves high thermal stability, Simple method and low cost effect

Active Publication Date: 2006-12-13
UNIV OF ELECTRONICS SCI & TECH OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The existing phthalonitrile resin with triazine ring structure has the disadvantages of low cross-linking degree and too much unreacted CN, which will easily lead to poor performance of the cured product and large high-temperature creep.
Its preparation synthetic method also still exists, adopts direct high-temperature melting reaction, makes reaction mechanism complicated, the deficiencies such as poor controllability

Method used

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  • Double end-group phthalonitrile, resin, condensate and its preparation method and uses
  • Double end-group phthalonitrile, resin, condensate and its preparation method and uses
  • Double end-group phthalonitrile, resin, condensate and its preparation method and uses

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] Embodiment 1 Preparation of double-terminated phthalonitrile monomer, phthalonitrile resin and cured product thereof of the present invention

[0050] 1. Synthesis of biphenyl-type double-terminated phthalonitrile monomer

[0051] 4-Nitrophthalonitrile 2mole

[0052] Biphenol 1mole

[0053] Anhydrous Potassium Carbonate 1.1mole

[0054] Add 30 moles of 4-nitrophthalonitrile, biphenol, anhydrous potassium carbonate, and solvent dimethylformamide into a four-necked bottle, feed nitrogen to replace the air therein, raise the temperature, and React at 85°C for 5 hours to stop the reaction, pour the reaction mixture into water to precipitate, add dilute hydrochloric acid to acidify, filter, wash with water three times, and dry in a vacuum oven at 80°C for 24 hours to obtain double-terminated biphenyl phthalonitrile .

[0055] After testing, the obtained biphenyl phthalonitrile monomer has a melting point of 227°C and a DSC curing peak temperature of 285°C.

[0056] 2. P...

Embodiment 2

[0064] Embodiment 2 Preparation of double-terminated phthalonitrile, phthalonitrile resin and cured product thereof of the present invention

[0065] 1. Synthesis of double-terminated biphenyl-type phthalonitrile

[0066] 4-Nitrophthalonitrile 2mole

[0067] Biphenol 1mole

[0068] Anhydrous sodium carbonate 1.5mole

[0069] Add 30 moles of 4-nitrophthalonitrile, biphenol, anhydrous sodium carbonate, and solvent dimethylacetamide into a four-necked bottle, feed nitrogen to replace the air therein, raise the temperature, and React at 80°C for 8 hours to stop the reaction, pour the reaction mixture into water to precipitate, add dilute hydrochloric acid to acidify, filter, wash with water three times, and dry in a vacuum oven at 80°C for 24 hours to obtain double-terminated biphenyl phthalonitrile.

[0070] After testing, the melting point of the biphenyl-type phthalonitrile monomer is 227°C, and the DSC curing peak temperature is 285°C;

[0071] 2. Preparation of phthalonit...

Embodiment 3

[0080] Example 3 Preparation of double-terminated phthalonitrile monomer, phthalonitrile resin and cured product thereof of the present invention

[0081] 1. Synthesis of double-terminated biphenyl-type phthalonitrile monomer

[0082] 4-Nitrophthalonitrile 2mole

[0083] Biphenol 1mole

[0084] Anhydrous potassium carbonate and anhydrous sodium carbonate (molar ratio 1 / 1) total 1.2mole

[0085] Add 30 moles of 4-nitrophthalonitrile, biphenol, anhydrous potassium carbonate and anhydrous sodium carbonate (molar ratio 1 / 1), and solvent dimethylacetamide into a four-necked bottle, and pass into Replace the air with nitrogen, raise the temperature, react at 90°C for 4 hours to stop the reaction, pour the reaction mixture into water to precipitate, add dilute hydrochloric acid to acidify, filter, wash with water three times, and dry in a vacuum oven at 80°C for 24 hours to obtain Double-terminated biphenyl phthalonitrile.

[0086] After testing, the melting point of the phthalon...

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Abstract

The invention belongs to the high molecular synthetic material field. The invention relates the double-end phthalonitrile, resin, condensate, which are made by phthalonitrile, and preparing method. The invention uses 4-nitro-o-phthalonitrile and dihydric phenol as reaction integral to get double-end phthalonitrile. The double-end phthalonitrile and diamine are used to react in aromatic amine solution at 140-200Deg.C to get phthalonitrile resin which possesses phthalocyanine ring structure. The resin is cured at 220-280Deg.C, then carried out heat treatment at 320-370Deg.C to get phthalocyanine condensate which possesses high heat stability. The invention has the advantages of good heat stability and fire-retardancy.

Description

technical field [0001] The invention belongs to the field of polymer synthetic materials, and in particular relates to a double-terminated phthalonitrile, a resin prepared from it as a raw material, a cured product, a preparation method and an application thereof. Background technique [0002] Phthalonitrile polymer is a new type of thermosetting polymer material, and it is a high-temperature-resistant polymer material with great application potential in the fields of aerospace, ships, and electronic packaging materials. It can prepare functional polymer materials, paints / coatings, resin-based composite materials, high-temperature-resistant adhesives, electronic conductors, semiconductors, organic magnetic functional materials, and has functional characteristics such as corrosion resistance, radiation resistance, and high strength. The existence of these performance and functional characteristics makes it have a wide range of application prospects. [0003] The development ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C43/275C08G69/38
Inventor 刘孝波李文婷罗道文陈文瑾何毅龙盛如曹国萍
Owner UNIV OF ELECTRONICS SCI & TECH OF CHINA
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