Preparation method of hexaaniline cyclotriphosphazene and non-halogen flame retardant epoxy resin composition

A technology based on cyclotriphosphazene and hexachlorocyclotriphosphazene, which is applied in the field of polymer composite material preparation, can solve the problems of increased viscosity of epoxy resin composite materials, corrosion of metal wires, reduced reliability and the like, and achieves flame retardant performance improved effect

Inactive Publication Date: 2009-12-09
GUANGDONG RONGTAI IND +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the flame retardant effect of hydroxide is poor, and a large amount needs to be added, which will increase the viscosity of the epoxy resin composite (EMC) and make it difficult to release the mold, causing packaging defects
When red phosphorus or phosphate is used, when packaged components are exposed to hot and humid environments, the phosphoric acid generated can cause corrosion of metal leads and reduce their reliability

Method used

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  • Preparation method of hexaaniline cyclotriphosphazene and non-halogen flame retardant epoxy resin composition
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  • Preparation method of hexaaniline cyclotriphosphazene and non-halogen flame retardant epoxy resin composition

Examples

Experimental program
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Embodiment 1

[0018] The embodiment of the present invention provides a preparation method of hexaanilinocyclotriphosphazene, the method comprising:

[0019] Add organic solvent, hexachlorocyclotriphosphazene, aniline, and acid-binding agent into the reaction device, stir, pass in nitrogen gas (nitrogen with a purity of not less than 99.9%) for protection, heat to 50-120°C, and then feed the reaction device Add tetrabutylammonium bromide catalyst, react for 5 to 16 hours, cool to room temperature, filter with suction, distill the filtrate under reduced pressure, evaporate and remove the solvent, and obtain a brown viscous product, which is placed in a drying box. After drying at 40-70° C. under vacuum for 8 hours, the powder product obtained by crushing is hexaanilinocyclotriphosphazene.

[0020] The structural formula of the hexaanilinocyclotriphosphazene made is:

[0021]

[0022] The solvent used in the above-mentioned method for preparing hexaanilinocyclotriphosphazene is any one or...

Embodiment 2

[0027] This example provides a method for preparing an epoxy resin composition using hexaanilinocyclotriphosphazene, mainly using the hexaanilinocyclotriphosphazene prepared in Example 1 to prepare a halogen-free flame-retardant epoxy resin Composition, the method specifically comprises:

[0028] The hexaanilinocyclotriphosphazene and o-cresol novolac epoxy resin, spherical silicon micropowder, imidazole curing accelerator, silane coupling agent, toughening agent and stearic acid prepared by the preparation method in the above-mentioned embodiment one The halogen-free flame-retardant epoxy resin composition is obtained after mixing the raw materials of the lubricant or wax lubricant, kneading, crushing, and degaussing treatment. Wherein, the mass proportion of hexaanilinocyclotriphosphazene and epoxy resin, curing agent, curing accelerator, silicon micropowder, lubricant, toughening agent and stearic acid is:

[0029] 10-30 parts by mass of o-cresol novolac epoxy resin

[00...

Embodiment 3

[0044] The present embodiment provides a kind of preparation method of hexaanilinocyclotriphosphazene, specifically comprises the following steps:

[0045]Take 5g of hexachlorocyclotriphosphazene and 80mL of tetrahydrofuran into a 250mL three-necked flask, add 12mL of triethylamine, fully stir and reflux, control the temperature of the water bath at 75°C, slowly add 8mL of aniline and 0.02g of tetrabutyl bromide Amine mixed solution, after reacting for 13h, was cooled to room temperature, obtained light yellow solution by suction filtration with vacuum pump, carried out normal pressure distillation to light yellow solution, removed solvent, obtained brown viscous thing, this material was placed in the vacuum oven (vacuum degree is less than -0.09MPa), dried at 60°C for 8 hours, and pulverized to obtain a brown powder product which is hexaanilinocyclotriphosphazene, with a yield of 80.2%.

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Abstract

The invention discloses a preparation method of hexaaniline cyclotriphosphazene and non-halogen flame retardant epoxy resin composition. The preparation method of hexaaniline cyclotriphosphazene comprises the following steps: adding solvent, hexachlorocyclotriphosphazene, aniline and acid-binding agent into a reaction device, stirring and introducing nitrogen for protection, heating the mixture to 50-120 DEG C, adding catalyst into the reaction device, reacting for 5-16h and cooling to room temperature, filtering, carrying out reduced pressure distillation on the filtrate, carrying out evaporation to remove solvent to obtain brown thick product, placing the product in a drying oven, drying for 8h in vacuum at 40-70 DEG C, crushing to obtain powder product, namely the hexaaniline cyclotriphosphazene. The non-halogen flame retardant epoxy resin composition applied to large-scale and very-large-scale integrated circuits encapsulation is prepared by mixing the prepared hexaaniline cyclotriphosphazene with o-cresol formaldehyde epoxy resin, microsilica, curing catalyst, silane coupling agent, lubricant, flexibilizer and stearic acid, milling, crashing and demagnetizing.

Description

technical field [0001] The invention relates to the field of polymer composite material preparation, in particular to a preparation method of a hexaanilinocyclotriphosphazene and a halogen-free flame-retardant epoxy resin composition. Background technique [0002] Epoxy resin has excellent physical and mechanical properties and electrical properties, and has a good cost performance ratio, so it is widely used as coatings, adhesives, composite resin matrix, electronic packaging materials, etc. In particular, epoxy resins have played a significant role in the packaging of electronic components and integrated circuits (ICs). At present, more than 95% of electronic components and integrated circuits are packaged with epoxy composite materials (EMC). The matrix resin used is mainly o-cresol novolac epoxy resin, and the filler used is mainly silicon micropowder. [0003] At present, the development trend of packaging technology is: packaging is developing in the direction of sma...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/6593C08L63/04C08L61/14C08K13/02C08K5/5399
Inventor 杨明山李林楷丁洁羽信全罗海平刘阳
Owner GUANGDONG RONGTAI IND
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