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A kind of phosphorus-containing flame-retardant epoxy resin modified by epoxy silicone oil and preparation method thereof

A technology of epoxy silicone oil and epoxy resin, which is applied in the field of preparation of epoxy silicone oil hydrophobically modified phosphorus-containing flame retardant epoxy resin, can solve the problem of accelerated aging of epoxy resin, electrical breakdown of epoxy resin parts, and inapplicability and other problems, to achieve the effect of excellent compatibility

Active Publication Date: 2018-08-17
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 also be seriously deteriorated.
Therefore, the existing DOPO-type phosphorus-containing flame-retardant epoxy resin is not suitable for outdoor or humid environments

Method used

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  • A kind of phosphorus-containing flame-retardant epoxy resin modified by epoxy silicone oil and preparation method thereof
  • A kind of phosphorus-containing flame-retardant epoxy resin modified by epoxy silicone oil and preparation method thereof
  • A kind of phosphorus-containing flame-retardant epoxy resin modified by epoxy silicone oil and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] 1) Add 5 g of epoxy silicone oil, 100 g of DOPO-type phosphorus-containing flame-retardant epoxy resin, 2 g of KH550 and 0.05 g of DBTL into a single-necked Erlenmeyer flask in turn, and react under vacuum at 80 °C for 2 h to obtain light yellow Uncured epoxy silicone oil modified phosphorus-containing flame-retardant epoxy resin (ESO-m-DE);

[0030] 2) Add 100 g of the obtained uncured epoxy silicone oil-modified phosphorus-containing flame-retardant epoxy resin, 50 g of phthalic anhydride and 0.4 g of N,N-dimethylbenzylamine into a polytetrafluoroethylene beaker , after heating and stirring at 40 ℃, pour it into the preheated mold, remove air bubbles in the oven, heat and cure at 100 ℃ for 3 hours, and then heat and cure at 130 ℃ for 10 hours. Cooling, demoulding and sampling, the finished product is obtained.

Embodiment 2

[0032] 1) Add 10 g of epoxy silicone oil, 120 g of DOPO-type phosphorus-containing flame-retardant epoxy resin, 3 g of KH550 and 0.08 g of DBTL into a single-necked Erlenmeyer flask in turn, and react under vacuum at 100 °C for 1 h to obtain light yellow Uncured epoxy silicone oil modified phosphorus-containing flame-retardant epoxy resin (ESO-m-DE);

[0033]2) Add 120 g of the obtained uncured epoxy silicone oil-modified phosphorus-containing flame-retardant epoxy resin, 70 g of methyltetrahydrophthalic anhydride and 0.6 g of N-benzylpyrazinium hexafluoroantimonate Put it into a polytetrafluoroethylene beaker, heat and stir at 60 °C and mix evenly, pour it into a preheated mold, remove air bubbles in an oven, heat and cure at 120 °C for 2 hours, and then heat and cure at 150 °C for 8 hours. After curing, the cured product is cooled with the furnace, demolded and sampled to obtain the finished product.

Embodiment 3

[0035] 1) Add 20 g of epoxy silicone oil, 140 g of DOPO-type phosphorus-containing flame-retardant epoxy resin, 4 g of KH550 and 0.1 g of DBTL into a single-necked Erlenmeyer flask in turn, and react under vacuum at 120 °C for 0.5 h to obtain light yellow Uncured epoxy silicone oil modified phosphorus-containing flame-retardant epoxy resin (ESO-m-DE);

[0036] 2) Add 140 g of the obtained uncured epoxy silicone oil-modified phosphorus-containing flame-retardant epoxy resin, 90 g of hexahydrophthalic anhydride and 0.8 g of N,N-dimethylbenzylamine into a polytetrafluoroethylene beaker, 80 After heating and stirring at ℃ and mixing evenly, pour it into a preheated mold, remove air bubbles in an oven, and then heat-preserve and cure at 140°C for 1 hour, and then heat-preserve and cure at 170°C for 6 hours. After curing, the cured product is cooled with the furnace. Demoulding and sampling, the finished product is obtained.

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Abstract

The invention discloses epoxy silicone oil modified phosphorus-containing flame-retardant epoxy resin and a preparation method thereof, belonging to the preparation field of high-performance high-polymer materials. According to the preparation method, epoxy silicone oil is taken as a water repellent agent, KH550 is taken as a compatilizer, and the epoxy silicone oil, KH550 and DOPO-type phosphorus-containing flame-retardant epoxy resin are connected together through chemical bonding by virtue of a vacuum stirring manner and are cured so as to prepare the epoxy silicone oil modified phosphorus-containing flame-retardant epoxy resin. The obtained epoxy silicone oil modified phosphorus-containing flame-retardant epoxy resin has excellent compatibility, hydrophobicity, flame retardance and mechanical properties, the vertical burning grade reaches the V-0 level, a surface contact angle is increased to 95.1-99.3 degrees, the tensile strength is 41.5-55.5MPa, and the impact strength is 2.7-14.6kJ / m<2>; and meanwhile, the epoxy resin has the characteristics of no toxicity and environmental friendliness, can be applied to outdoor or moist 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 epoxy silicone oil 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, coatings, and 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 resins, people add organophosphorus flame retardants to epoxy resins to prepare DOPO type epoxy resins with excellent flame retardancy and low toxicity, or even non-toxicity. However, the epoxy resin itself is highly polar and does not have hydrophobicity. Adding an organic phosphorus flame retardant will fu...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G59/14C08G59/42C08G59/68
CPCC08G59/1438C08G59/4223C08G59/686
Inventor 李宝铭林立百梦弟
Owner FUZHOU UNIV
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