Magnetic ferrocene-double-terminal phthalonitrile resin, condensate and preparation thereof

A kind of base phthalonitrile resin, the technology of base phthalonitrile, applied in cured product and their preparation, the field of magnetic ferrocene-double-end phthalonitrile resin, can solve the problem of synthetic magnetic ferrocene - double-end phthalonitrile resin and other problems, to achieve the effects of controllable reaction process and structure, good magnetic properties, simple and effective method

Inactive Publication Date: 2009-06-24
UNIV OF ELECTRONICS SCI & TECH OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] So far, there is no report on the synthesis of magnetic ferrocene-two-terminal phthalonitrile resin and its cured product

Method used

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  • Magnetic ferrocene-double-terminal phthalonitrile resin, condensate and preparation thereof
  • Magnetic ferrocene-double-terminal phthalonitrile resin, condensate and preparation thereof
  • Magnetic ferrocene-double-terminal phthalonitrile resin, condensate and preparation thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] (1) Preparation of magnetic ferrocene-two-terminal phthalonitrile resin

[0035] Raw material consumption is (by mol):

[0036] Ferrocene formaldehyde 4

[0037] Biphenol 1

[0038] 4-(4-Aminophenoxy)phthalonitrile 2

[0039] N,N-Dimethylformamide 15

[0040] Ferrocene formaldehyde, 4-(4-aminophenoxy) phthalonitrile, biphenol and N, N-dimethylformamide are added in the four-necked bottle according to the above-mentioned mol ratio, and passed into Nitrogen was used to replace the air in it, and the temperature was raised to 90-100° C. for 6 hours, and nitrogen was used to protect the whole reaction process. Pour the reaction mixture into 0.1M / L NaOH solution to precipitate, filter, and wash the obtained solid with ethanol several times, then place it in a vacuum oven and dry it at 60°C for 24 hours to obtain the magnetic ferrocene-double-terminal phthalate Dicyanonitrile resin, yield 73%, curing peak temperature is double curing peak, respectively 221 ° C and 262.2 ...

Embodiment 2

[0051] The preparation method is the same as in Example 1, except that the iron trichloride in the step (2) is changed to ferric nitrate, and the properties of the magnetic ferrocene-two-end phthalonitrile resin prepared are as follows: yield 74.1%, The curing peak temperature is a double curing peak, respectively 221.3°C and 263.2°C, and the FTIR spectrum shows a 945cm -1 The characteristic absorption peak of the benzoxazine ring, 2225cm -1 The characteristic absorption peak of the nitrile group.

[0052] The properties of the cured resin obtained are as follows: the saturation magnetization of the cured product is 1.95575emu / g, the residual magnetism reaches 0.12012emu / g, and the coercive force is 73.310e. The Curie temperature is above 500K. The glass transition temperature is 313°C; the decomposition temperature (5%) is 422°C; and the carbon residue rate in nitrogen atmosphere at 800°C is 71.4%.

Embodiment 3

[0054]The preparation method is the same as in Example 1, except that N, N-dimethylformamide in step (1) is replaced with N-methylpyrrolidone, and the magnetic ferrocene-two-end phthalonitrile resin obtained has the following properties : Yield 74.7%, DSC curing peak temperature is double curing peak, respectively 222.3 ℃ and 264.2 ℃, FTIR spectrum shows 945cm -1 The benzoxazine ring characteristic, 2225cm -1 There are characteristic absorptions of nitrile groups.

[0055] The properties of the cured resin obtained are as follows: the saturation magnetization of the cured product is 1.98375emu / g, the residual magnetism reaches 0.12852emu / g, and the coercive force is 74.210e. The Curie temperature is above 500K. The glass transition temperature is 315°C; the decomposition temperature (5%) is 424°C; the carbon residue rate in nitrogen atmosphere at 800°C is 72.4%.

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Abstract

The invention belongs to the high molecular material field, in particular to magnetic ferrocene-double terminal phthalonitrile resin, a cured product and a preparation method thereof. The structure of the magnetic ferrocene-double terminal phthalonitrile resin is as shown in formula I. The magnetic ferrocene-double terminal phthalonitrile resin and ferric iron salt react in an anhydrous and highly polar solvent at the temperature of 150-170 DEG C, then are washed and dehydrated to obtain a prepolymer, and the prepolymer is heated to 190-210 DEG C for precuring for 2-4h, and then heated to 340-360 DEG C for heat treatment for 4-6h to obtain the cured product of the resin. The resin prepared by the method has a wider processing temperature window, simple reaction process and easy operation; and the cured product has abundant crosslinking structures, better thermostability and magnetism, and can be widely applied to high temperature resistant magnetic functional composite materials.

Description

technical field [0001] The invention belongs to the field of polymer materials, and in particular relates to magnetic ferrocene-double-end phthalonitrile resins, cured products and their preparation methods. Background technique [0002] Since Kealy and Pauson synthesized ferrocene in 1951, its unique aromatic sandwich structure and the chemical properties of the central iron element have made it widely used in many fields, such as asymmetric catalysis, nonlinear optics, and electrochemistry. Metal-organic polymers based on ferrocene give full play to the unique properties of ferrocene in terms of light, electricity, and magnetism. According to the different positions of ferrocene in the polymer chain structure, ferrocene-based polymers can be divided into three categories: one is the main chain type; the other is the side chain type, including the formation of ferrocene in the same ring The polymer; the third is a dendritic or hyperbranched type. At present, side-chain fe...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F17/02C08G79/00C08G73/06
Inventor 魏俊基贾坤钟家春赵睿刘孝波
Owner UNIV OF ELECTRONICS SCI & TECH OF CHINA
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