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Diamine-triphenol type hyperbranched polybenzoxazine and preparation method thereof

A polybenzoxazine, phenol type technology, applied in the field of organic polymer materials, can solve the problems of high curing temperature, poor toughness, low cross-linking density, etc. Effect

Active Publication Date: 2019-10-11
HARBIN ENG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, benzoxazine has the disadvantages of low crosslinking density, high curing temperature and poor toughness, so it is necessary to modify it

Method used

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  • Diamine-triphenol type hyperbranched polybenzoxazine and preparation method thereof
  • Diamine-triphenol type hyperbranched polybenzoxazine and preparation method thereof
  • Diamine-triphenol type hyperbranched polybenzoxazine and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] In a three-necked flask equipped with a magnetic stirring rotor, a thermometer and a condenser, add trisphenolyl methane (0.78g, 2mmol), polyetheramine D-230 (0.69g, 3mmol), paraformaldehyde (0.36g, 12mmol) and 50mL of 1,4-dioxane solvent, heated up to 100°C, and reacted at a constant temperature for 72h, the reaction solution was washed with 0.2mol / L NaOH solution, washed with water, rotary evaporated, and dried in vacuum to obtain polyetheramine D- 230-trisphenol-based methyl hyperbranched polybenzoxazine powder, the yield is 83%, the weight average molecular weight of the polymer is 36000, and the PDI is 3.2.

[0021] Proton NMR spectrum test results (500M, DMSO-d 6 , ppm): 6.65-7.28ppm is the chemical shift of the proton hydrogen on the benzene ring; 5.34ppm and 4.88ppm are the O-CH on the oxazine ring 2 -N and Ar-CH 2 The characteristic peak of -N; 3.74ppm is the chemical shift of amino proton hydrogen; 2.71ppm is the characteristic peak of methine proton hydroge...

Embodiment 2

[0024] Except that polyetheramine D-230 is replaced by ethylenediamine (0.18g, 3mmol), other conditions are the same as in Example 1, and finally ethylenediamine-trisphenol-methyl hyperbranched polybenzoxazine is obtained with a yield of 87 %, the weight average molecular weight of the polymer is 24500, and the PDI is 2.7.

[0025] Proton NMR spectrum test results (500M, DMSO-d 6 , ppm): 6.64~7.27, 5.32, 4.77, 3.83, 2.76, 0.98~1.03; infrared spectrum test results (KBr, cm -1 ): 3433, 2944, 2852, 1671, 1613, 1496, 820, 1330, 1231, 1118, 921, 872, 748, 701. Combined with H NMR and IR spectra, it was confirmed that the obtained product was the target product.

[0026] Curing and test condition are the same as embodiment 1, finally obtain the T g , T 5 , T 10 and Yc The values ​​were 231°C, 374°C, 398°C and 43.6%, respectively.

Embodiment 3

[0028] Except that the reaction time was changed from 72h to 48h, other conditions were the same as in Example 2, and finally ethylenediamine-trisphenol-methyl hyperbranched polybenzoxazine was obtained with a yield of 85%, and the weight-average molecular weight of the polymer was 19700. The PDI is 2.3.

[0029] Curing and test condition are the same as embodiment 1, finally obtain the T g , T 5 , T 10 and Y c The values ​​were 227°C, 367°C, 382°C and 39.8%, respectively.

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Abstract

The invention provides diamine-triphenol hyperbranched polybenzoxaizne and a preparation method thereof. The method comprises the steps of adding a diamine compound, a triphenol compound, paraformaldehyde and an organic solvent into a container, wherein the mass ratio of the diamine compound to the triphenol compound to paraformaldehyde is 3:2:12; and heating to 60-110 DEG C, carrying out thermostatic reaction for 10-75h, carrying out alkali washing on a reaction liquid through a 0.2mol / L NaOH solution and carrying out water washing, rotary evaporation and vacuum drying to obtain diamine-triphenol hyperbranched polybenzoxaizne, wherein the weight-average molecular weight of the product is 6,000-55,000 and the molecular weight distribution index is 1.7-3.5. Diamine-triphenol hyperbranched polybenzoxaizne is synthesized from the triphenol compound and the diamine compound. Due to a plurality of oxazine rings, the curing product is high in crosslinking density and high in molecular weight, has excellent thermal property and mechanical property, can be used for preparing a high-performance structure material and an electronic packaging material, and can be widely applied to the fields of electronics, aviation, machinery manufacturing and etc.

Description

technical field [0001] The invention relates to an organic polymer material, and also relates to a preparation method of the organic polymer material. Specifically, it relates to a diamine-triphenol type hyperbranched polybenzoxazine and a preparation method thereof. Background technique [0002] Benzoxazine is a six-membered heterocyclic compound containing O and N atoms formed by condensation of phenolic compounds, primary amine compounds and formaldehyde (or paraformaldehyde) through Mannich reaction. Under the action of heating or catalyst, benzoxazine can be ring-opened and polymerized to form a cross-linked network structure similar to phenolic resin. Compared with traditional phenolic resins, benzoxazine has superior performance, flexible molecular design, no need to use strong acid or alkali as a catalyst in the curing process, no small molecular by-products are generated, and the volume is approximately zero shrinkage or even slightly Swelling, polymers have high ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G14/06
Inventor 刘文彬蔡万安王军宋莎桑梓
Owner HARBIN ENG UNIV
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