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Benzoxazine resin intermediate, resin and solidified matter and their preparing method and use

A resin cured product, benzoxazine technology, applied in the field of benzoxazine intermediates, benzoxazine intermediates and prepared resins, to achieve good curing reactivity, good mechanical strength, high thermal stability Effect

Inactive Publication Date: 2007-01-24
UNIV OF ELECTRONICS SCI & TECH OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Chinese invention patents CN99114603.4, CN03126518.9, CN02108772.5, CN03146797.0, CN02806290.6, etc. have invented the preparation method of benzoxazine intermediates and resins and their applications in laminates and coatings. Based on phenol, aldehyde and amine component compounds, no cyanodiamines have been used as raw materials to prepare benzoxazine resins, and cyano-containing benzoxazine monomers have only been reported on p-aminobenzonitrile

Method used

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  • Benzoxazine resin intermediate, resin and solidified matter and their preparing method and use
  • Benzoxazine resin intermediate, resin and solidified matter and their preparing method and use
  • Benzoxazine resin intermediate, resin and solidified matter and their preparing method and use

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Embodiment 1

[0038] Preparation and physicochemical properties of embodiment 1 benzoxazine intermediate of the present invention

[0039] (1) Raw material ratio for preparing cyano side group diamine:

[0040] 218 grams of p-aminophenol, 172 grams of 2,6-dichlorobenzonitrile, and 151 grams of catalyst potassium carbonate.

[0041] (2) Preparation of cyano pendant diamines: Add p-aminophenol, 2,6-dichlorobenzonitrile, catalyst, anhydrous dimethylformamide, and toluene to a four-necked bottle with water separator , pass nitrogen to replace the air in it, raise the temperature, react at 140°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, the cyano pendant diamine was obtained with a yield of 96%.

[0042] (3) Raw material ratio for preparing benzoxazine intermediate:

[0043] Take 188 grams of phenol, 400 grams of 30% w / w form...

Embodiment 2

[0046] Embodiment 2 Preparation and physicochemical properties of benzoxazine intermediate of the present invention

[0047] (1) Raw material ratio for preparing cyano side group diamine:

[0048] 218 grams of p-aminophenol, 172 grams of 2,6-dichlorobenzonitrile, and 115 grams of catalyst sodium carbonate.

[0049] (2) Preparation of cyano side group diamine: p-aminophenol, 2,6-dichlorobenzonitrile, catalyzer, dimethylacetamide, dimethylbenzene are added in the four-necked bottle with water separator, Introduce nitrogen to replace the air in it, raise the temperature, react at 160°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 cyano pendant diamine with a yield of 97%.

[0050] (3) Raw material ratio for preparing benzoxazine intermediate:

[0051] 317 grams of cyano pendant diamines, 188 gr...

Embodiment 3

[0054] Embodiment 3 Preparation and physicochemical properties of benzoxazine intermediate of the present invention

[0055] (1) Raw material ratio for preparing cyano side group diamine:

[0056] 218 grams of p-aminophenol, 172 grams of 2,6-dichlorobenzonitrile, and 151 grams of catalyst potassium carbonate.

[0057] (2) Preparation of cyano side group diamine: p-aminophenol, 2,6-dichlorobenzonitrile, catalyzer, dimethylacetamide, dimethylbenzene are added in the four-necked bottle with water separator, Introduce nitrogen to replace the air in it, raise the temperature, react at 140°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 cyano pendant diamine with a yield of 96.5%.

[0058] (3) Raw material ratio for preparing benzoxazine intermediate:

[0059] 317 grams of pendant cyano diamines, 188 grams...

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Abstract

The present invention provides benzoxazine resin intermediate prepared with diamine with side cyano radical, benzoxazine resin and benzoxazine resin condensate. The preparation process is simple and high in yield, and the benzoxazine resin and the benzoxazine resin condensate have good self fire retarding property, adhering property, heat stability and flowability, and may be applied widely in paint, electronic packaging material and resin base composite material.

Description

technical field [0001] The invention relates to a benzoxazine intermediate, in particular to a benzoxazine intermediate and a prepared resin, and belongs to the field of polymer material synthesis. Background technique [0002] Benzoxazine resin is an intermediate prepared from a compound containing a benzoxazine ring structure (called a benzoxazine intermediate), through which a polymer resin is prepared. The benzoxazine resin can be further reacted to form a material called "benzoxazine material", which has a typical characteristic absorption at 945cm-1 on FTIR. Due to the different structures of the intermediates, the final resin and post-product structures of this kind of resin are different, resulting in different physical and chemical characteristics, performance and functions; the preparation process is mainly due to the different ways of adding raw materials, or using different reaction methods, such as solution reaction, dispersion reaction, Suspension dispersion r...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D265/14C08G73/06C08L69/00C09K3/10C09D179/00
Inventor 陈文瑾曹国萍刘孝波罗道文何毅龙盛如
Owner UNIV OF ELECTRONICS SCI & TECH OF CHINA