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 resin, achieve improved performance, simple preparation method, The effect of low curing temperature

Active Publication Date: 2014-04-09
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
Comparison scheme
Effect test

Embodiment 1

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

Embodiment 2

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

Embodiment 3

[0052] In a 100ml round-bottomed flask equipped with a condenser, add monoaminoethylferrocene (0.105mol, 24.045g), m-cresol (0.105mol, 11.34g), paraformaldehyde (0.21mol, 6.3g), Then add 28.20 ml of chloroform, stir electromagnetically, heat at 90 °C for 3 h, cool down to room temperature, use 3 mol / L NaHCO 3 The chloroform solution containing the product was washed once with an aqueous solution, and then washed with pure water until neutral. The solvent was removed by rotary evaporation under reduced pressure and dried to obtain a ferrocene-containing benzoxazine monomer. The ferrocene-based benzoxazine monomer is cured under a temperature-programmed curing process to obtain a ferrocene-based benzoxazine resin. The specific curing process is: 60 ℃ 1h + 90 ℃ 1h + 130 ℃ 1h + 180 ℃ 1h + 230℃ 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 present invention relates to a ferrocenyl-containing benzoxazine monomer or precursor and a method for preparing the monomer or precursor, and a ferrocenyl-containing benzoxazine formed by thermal curing of 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 is usually synthesized from phenol, formaldehyde and primary amine compounds to obtain monomers or precursors, and then the monomers or precursors are obtained by ring-opening polymerization 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 release of small molecules during cu...

Claims

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Application Information

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Patent Type & Authority Patents(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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