Preparation of ferrocenyl benzoxazine-containing monomer or precursor and heat reactive resin thereof

A ferrocene-based benzene and precursor technology, applied in metallocene, organic chemistry, chemical instruments and methods, etc., can solve problems such as reducing the temperature resistance of benzoxazine resins, and achieve improved performance, low curing temperature, High temperature resistance and effect of electromagnetic properties

Active Publication Date: 2012-02-15
NANJING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Takechi et al. have attempted to add transition metal compounds of acetyl ligands to benzoxazine resins, and studied the effect of the transition metal complexes on the curing temperature and temperature resistance of benzoxazine resins. The results show that the transition Metal complexes can effectively promote the curing of benzoxazine resins, but reduce the temperature resistance of benzoxazine resins【Journal of Polymer Science: Part A: Polymer Chemistry, 2010; 48: 479—484】

Method used

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  • Preparation of ferrocenyl benzoxazine-containing monomer or precursor and heat reactive resin thereof
  • Preparation of ferrocenyl benzoxazine-containing monomer or precursor and heat reactive resin thereof
  • Preparation of ferrocenyl benzoxazine-containing monomer or precursor and heat reactive resin thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0048] In a 100ml round bottom flask equipped with a condenser, add monoaminoferrocene (0.01mol, 2.01g), phenol (0.011mol, 1.034g), paraformaldehyde (0.022mol, 0.66g), and then add chloroform 50.12 ml, electromagnetically stirred, heated at 60°C for 24 hours, cooled to room temperature, washed the chloroform solution containing the product once with 0.1 mol / L NaOH aqueous solution, and then washed with pure water until neutral. The solvent was removed by rotary evaporation under reduced pressure, and the ferrocenyl-containing benzoxazine monomer was obtained by drying. The ferrocenyl benzoxazine monomer is cured under a temperature-programmed curing process to obtain a ferrocenyl benzoxazine resin. The specific curing process is: 60°C 1h + 100°C 1h + 140°C 1h + 200°C °C 1h + 240°C 1h.

Embodiment 2

[0050] In a 100ml round bottom flask equipped with a condenser, add monoaminomethylferrocene (0.11mol, 23.65g), p-cresol (0.10mol, 10.80g), paraformaldehyde (0.22mol, 6.6g), Then add 55.55ml of chloroform, stir electromagnetically, heat the reaction at 110°C for 12h, cool down to room temperature, and use 5mol / L Na 2 CO 3 The chloroform solution containing the product was washed once with aqueous solution, and then washed with pure water until neutral. The solvent was removed by rotary evaporation under reduced pressure, and the ferrocenyl-containing benzoxazine monomer was obtained by drying. The ferrocenyl benzoxazine monomer is cured under a temperature-programmed curing process to obtain a ferrocenyl benzoxazine resin. The specific curing process is: 60°C 1h + 80°C 1h + 120°C 1h + 170°C °C 1h + 220°C 1h.

Embodiment 3

[0052] In a 100ml round bottom flask equipped with a condenser, add monoaminoethylferrocene (0.105mol, 24.045g), m-cresol (0.105mol, 11.34g), paraformaldehyde (0.21mol, 6.3g), Then add 28.20ml of chloroform, electromagnetically stir, heat the reaction at 90°C for 3h, cool down to room temperature, and use 3mol / L NaHCO 3 The chloroform solution containing the product was washed once with aqueous solution, and then washed with pure water until neutral. The solvent was removed by rotary evaporation under reduced pressure, and the ferrocenyl-containing benzoxazine monomer was obtained by drying. The ferrocenyl benzoxazine monomer is cured under a temperature-programmed curing process to obtain a ferrocenyl benzoxazine resin. The specific curing process is: 60°C 1h + 90°C 1h + 130°C 1h + 180°C °C 1h + 230°C 1h.

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Abstract

The invention discloses a ferrocenyl benzoxazine-containing monomer or precursor and its preparation method as well as a ferrocenyl benzoxazine-containing resin prepared by thermal curing of the monomer or precursor. The preparation method provided by the invention comprises the following steps of: mixing and dissolving 1-400 wt% of reactants and organic solvents in a reactor while the temperature is controlled within 40-130 DEG C and the reaction lasts for 0.5-24 hours; washing a purification product by the use of an alkaline solution at the concentration of 0.01mol/L-5mol/L, washing the product to neutral by the use of pure water, removing the organic solvents, and drying to prepare the ferrocenyl benzoxazine-containing monomer or precursor. The ferrocenyl benzoxazine-containing resin is obtained by the heating, ring-opening and curing molding of the monomer or precursor. The monomer or precursor has low curing temperature, has a self-catalysis curing function, is widely applied, and can undergo crossing and curing under the heating condition without a catalyst and with no release of micromolecules. The cured ferrocenyl benzoxazine-containing resin has high temperature resistance and electromagnetic properties, and has an application prospect in the aspects of high temperature ceramics, electrochemical induction, high dielectric materials, magnetic ceramic body and the like.

Description

technical field [0001] The invention relates to a ferrocenyl-based benzoxazine monomer or precursor and a preparation method of the monomer or precursor, and a ferrocenyl-based benzoxazine formed by thermosetting the monomer or precursor resin. Background technique [0002] Traditional phenolic resins are widely used because of their excellent temperature resistance, flame retardancy, mechanical strength, corrosion resistance and electrical insulation. As a new type of phenolic resin, polybenzoxazine resin can usually be synthesized from phenol, formaldehyde and primary amine compounds as raw materials to obtain monomers or precursors, and then ring-opening polymerization of monomers or precursors under heating conditions. . In addition to the general characteristics of traditional phenolic resins, polybenzoxazine also has characteristics that traditional phenolic resins do not have, such as molecular designability, no small molecule release during curing, no need for acid...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F17/02C08G73/00
Inventor 贾叙东李维智袭锴孟震高迎春韦腾
Owner NANJING UNIV
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