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Silane hydrophobically modified phosphorus-containing flame-retardant epoxy resin and preparation method thereof

An epoxy resin and hydrophobic modification technology, which is applied in the field of preparation of high-performance polymer materials, can solve problems such as accelerated aging of epoxy resin, flicker and partial discharge, and deterioration of mechanical properties, and achieve excellent compatibility, excellent resistance flammability effect

Active Publication Date: 2018-02-09
FUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Studies have found that in lightning weather, the residual water on the surface of the epoxy resin is likely to cause flicker and partial discharge, which can accelerate the aging of the epoxy resin, or cause electrical breakdown of the entire epoxy resin component.
In addition, water is also a craze initiator. If the epoxy resin is used in a high humidity environment for a long time, its mechanical properties will be seriously deteriorated.

Method used

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  • Silane hydrophobically modified phosphorus-containing flame-retardant epoxy resin and preparation method thereof
  • Silane hydrophobically modified phosphorus-containing flame-retardant epoxy resin and preparation method thereof
  • Silane hydrophobically modified phosphorus-containing flame-retardant epoxy resin and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Add 40 g of DOPO-VTS, 100 g of DOPO-type epoxy resin, 0.8 g of dibutyltin dilaurate (DBTL) and 4 g of deionized water into a 250 mL round-bottomed flask equipped with a condenser, and stir at 80 °C for 6 h , and then evacuated for 2 h to obtain a yellow colloidal silane hydrophobically modified phosphorus-containing flame-retardant epoxy resin (DV-m-DE).

[0023] Add 100 g DV-m-DE, 50 g methyltetrahydrophthalic anhydride and 0.4 g N,N-dimethylbenzylamine into a polytetrafluoroethylene beaker, heat and stir at 40 °C to mix evenly, then pour Put it into a preheated mold, put it into a vacuum oven to remove air bubbles, and then heat up and solidify. The curing conditions are: 100°C for 3 hours, 130°C for 10 hours, and the cured product is cooled in the furnace, and then demoulded and sampled.

[0024] The vertical combustion grade of the epoxy resin reaches V-0 grade, and the surface contact angle is 106.3°.

Embodiment 2

[0026] Add 20 g of DOPO-VTS, 150 g of DOPO-type epoxy resin, 1.6 g of dibutyltin dilaurate (DBTL) and 0.5 g of deionized water into a 250 mL round bottom flask equipped with a condenser, and stir at 110 °C for 2 h, and then evacuated for 0.5 h to obtain a yellow colloidal silane hydrophobically modified phosphorus-containing flame-retardant epoxy resin (DV-m-DE).

[0027] Add 140 g DV-m-DE, 90 g hexahydrophthalic anhydride and 0.8 g N-benzylpyrazine sodium hexafluoroantimonate into a polytetrafluoroethylene beaker, heat and stir at 80 °C to mix evenly, then pour into the preheated Put it into a vacuum oven to remove air bubbles, then heat up and solidify; the curing conditions are: 140 °C for 1 h, 170 °C for 6 h, and the cured product is cooled in the furnace, and then demolded and sampled.

[0028] The vertical combustion grade of the epoxy resin reaches V-0 grade, and the surface contact angle is 92.7°.

Embodiment 3

[0030] Add 30 g of DOPO-VTS, 130 g of DOPO-type epoxy resin, 1.2 g of dibutyltin dilaurate (DBTL) and 2 g of deionized water into a 250 mL round bottom flask equipped with a condenser, and stir at 100 °C for 4 h , and then vacuum reaction for 1h to obtain yellow colloidal silane hydrophobically modified phosphorus-containing flame-retardant epoxy resin (DV-m-DE).

[0031] Add 120 g DV-m-DE, 70 g 3,4,5,6-tetrahydrophthalic anhydride and 0.6 g N-benzylquinoline sodium hexafluoroantimonate into a polytetrafluoroethylene beaker, 60 After heating and stirring at ℃ and mixing evenly, pour it into a preheated mold, put it in a vacuum oven to remove air bubbles, and then heat up and solidify. The curing conditions are: 120 ℃ for 2 hours, 150 ℃ for 8 hours. Sample demoulding.

[0032] The vertical combustion grade of the epoxy resin reaches V-0 grade, and the surface contact angle is 97.1°.

[0033] from image 3 It can be seen that in the infrared absorption spectrum of DOPO-VTS, t...

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Abstract

The invention relates to a phosphorus-containing flame-retardant epoxy resin having undergone hydrophobic modification by silane, and a preparation method thereof, belonging to the field of preparation of high-performance high polymer materials. The preparation method comprises the following steps: adding 20 to 40 g of DOPO-VTS, 100 to 150 g of DOPO type epoxy resin, 0.8 to 1.6 g of dibutyltin dilaurate (DBTL) and 0.5 to 4 g of deionized water into a 250-mL round-bottom flask equipped with a condenser tube; carrying out a reaction at 80 to 110 DEG C under stirring for 2 to 6 h; and then carrying out a vacuumized reaction for 0.5 to 2 h so as to obtain the yellow gummy phosphorus-containing flame-retardant epoxy resin (DV-m-DE) having undergone hydrophobic modification by silane. The epoxy resin prepared in the invention has excellent hydrophobicity and flame resistance; the vertical combustion grade of the epoxy resin reaches V-0 grade; the surface contact angle of the epoxy resin is increased to 92.7 to 106.3 DEG; and the epoxy resin has the characteristics of excellent compatibility, nontoxicity and environment friendliness, can be applied to outdoor or wet severe environments and has wide application prospects.

Description

technical field [0001] The invention belongs to the field of preparation of high-performance polymer materials, and in particular relates to a preparation method of silane hydrophobically modified phosphorus-containing flame-retardant epoxy resin. Background technique [0002] Epoxy resin has good adhesion, mechanical properties, electrical insulation and chemical corrosion resistance, and is widely used in many fields such as electrical and electronic products, transportation equipment, and coating adhesives. However, the flame retardancy of ordinary epoxy resin is poor, and there is a serious fire hazard. In order to improve the flame retardancy of epoxy resin, halogen-containing flame retardants are often added, but due to the high toxicity of halogen-containing flame retardants, secondary hazards are likely to occur during the flame-retardant process. Therefore, people began to turn their attention from halogen-containing flame retardants to organophosphorus flame retar...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G59/14
CPCC08G59/1488
Inventor 李宝铭吴志胤彭恩凯
Owner FUZHOU UNIV
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