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Efficient flame retardant dispersion liquid for epoxy resin and preparation method thereof

A technology for epoxy resin and epoxy resin, which is applied in the field of flame retardants, can solve the problems of reduced thermal stability and poor solubility, and achieves improved thermal stability and mechanical properties, good miscibility, and simple preparation method. Effect

Active Publication Date: 2018-02-06
广州埃米石墨烯科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Recently, Qinqin Luo et al. (RSC Advances, 2015, 5:68476–68484) from South China University of Technology found that 5,10-dihydro-phosphazine-10-oxide (DPPA) and its derivatives are used in epoxy resin Flame retardant has a good effect. Adding 3.2 parts of DPPA can make the cured epoxy resin pass the UL 94V-0 level, but even at such a low dosage, the presence of such compounds will make the original epoxy resin The thermal stability of DPPA is reduced, and DPPA and its derivatives have poor solubility in epoxy resin prepolymers, so they need to be heated above 160°C to mix with epoxy resin evenly

Method used

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  • Efficient flame retardant dispersion liquid for epoxy resin and preparation method thereof
  • Efficient flame retardant dispersion liquid for epoxy resin and preparation method thereof
  • Efficient flame retardant dispersion liquid for epoxy resin and preparation method thereof

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Experimental program
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Effect test

Embodiment 1

[0027] Preparation of high-efficiency flame retardant dispersion for epoxy resin, the specific steps are as follows:

[0028] Preparation of 5,10-dihydro-phosphazine-10-oxide (DPPA) (refer to RSC Advances, 2015, 5:68476–68484): 51.0 g of diphenylamine was added to the flask, and 44.0 g of three Phosphorus chloride, stirred for 30 minutes, gradually raised the temperature to 210°C, continued to stir for 7 hours, cooled to room temperature, and obtained a solid substance; after pulverizing the solid substance, gradually added 100mL of distilled water, heated and refluxed for 1 hour, and then cooled to 80°C , add 800mL of ethanol and stir thoroughly, filter while hot, wait for the filtrate to cool to room temperature, add excess 10% sodium hydroxide solution under stirring, adjust the pH of the solution to 10, filter to remove the precipitate; distill the ethanol in the filtrate to obtain DPPA Crude product, after washing to neutrality, DPPA is recrystallized with glacial acetic ...

Embodiment 2

[0034] To prepare the high-efficiency flame retardant dispersion liquid for epoxy resin, the specific steps are as follows:

[0035] Preparation of graphite oxide: under an ice bath, add 1.0 g graphite, 4 g potassium permanganate, 25 g concentrated sulfuric acid with a mass concentration of 98% and 2.5 g phosphoric acid with a mass concentration of 85% in sequence, stir for 4 hours and then heat up to 55 ° C, the reaction 10h, then pour the reaction solution into 300mL ice water, add 10g of 30% hydrogen peroxide to react for 3h, centrifuge to separate the bottom solids; wash twice with 4% hydrochloric acid solution, and then deionize Washed with water until neutral, then filtered, and the obtained filter cake was dried in a vacuum drying oven at 55°C to obtain a yellow-brown solid product, namely graphite oxide;

[0036] The preparation of DPPA-coated graphene oxide dispersion: get 0.23g of above-mentioned graphite oxide and mix with 13.7g of absolute ethanol, add 2.27g of DPP...

Embodiment 3

[0039] To prepare the high-efficiency flame retardant dispersion liquid for epoxy resin, the specific steps are as follows:

[0040] Preparation of graphite oxide: under ice bath, add 1.0g graphite, 5g potassium permanganate, 20g concentrated sulfuric acid with a mass concentration of 98% and 3g phosphoric acid with a mass concentration of 85% in sequence, stir for 3 hours, then heat up to 65 ° C, and react for 12 hours , then poured the reaction solution into 250 mL of ice water, added 8 g of hydrogen peroxide with a mass concentration of 30%, reacted for 1 h, centrifuged, and collected the bottom solid; washed twice with a 4% mass concentration of hydrochloric acid solution, and then used deionized water Washed to neutrality, then filtered, and the obtained filter cake was dried in a vacuum drying oven at 60° C. to obtain a yellow-brown solid product, which was graphite oxide.

[0041] Preparation of DPPA-coated graphene oxide dispersion: get 0.44g of above-mentioned graphit...

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Abstract

The invention relates to an efficient flame retardant dispersion liquid for epoxy resin and a preparation method thereof. The efficient flame retardant dispersion liquid is prepared by dispersing graphite oxide in a solvent and compounding the same with a phosphorus azine compound; the phosphorus azine compound is 5,10-hydro-phosphorus azin-10-oxide and a derivative thereof. The consolute temperature of the efficient flame retardant dispersion liquid for epoxy resin provided by the invention with an epoxy resin prepolymer is low, and the epoxy resin system has an excellent flame retardant effect (the epoxy resin cured product passes a UL94 V0 grade when the dosage is 2.5 parts) under the condition of relatively less dosage, and the mechanical strength and the thermal stability of the epoxyresin are not influenced, or even are improved.

Description

technical field [0001] The invention relates to the technical field of flame retardants, in particular to a high-efficiency flame retardant dispersion suitable for epoxy resins and a preparation method thereof. Background technique [0002] Bisphenol A epoxy resin (commonly known as epoxy resin) has the advantages of excellent adhesion, electrical insulation, chemical resistance, high tensile strength, good product dimensional stability, etc., and is widely used as an adhesive Adhesives, anti-corrosion coatings, insulating materials, laminated materials, etc., are directly or indirectly used in almost all industrial fields, but their high flammability makes them a huge safety hazard in the application process. The addition of flame retardants can endow epoxy resins with a certain degree of flame retardancy. Halogen-free flame retardants are the current development direction, and phosphorus-based flame retardants have attracted widespread attention due to their high flame ret...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08K9/10C08K3/04C08J3/20C08L63/00
CPCC08J3/2053C08J2363/00C08K3/04C08K9/10C08L2201/02C08L2201/08C08L63/00
Inventor 范国强张敏黄晓明
Owner 广州埃米石墨烯科技有限公司
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