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Preparation method of epoxy resin/iron phenyl phosphate composite

A nano-composite material, phenyl iron phosphate technology, applied in the field of new materials, can solve the problem of further improvement of flame retardant efficiency, and achieve the effect of easy industrial production, cheap raw materials, and less addition

Active Publication Date: 2019-03-19
TECHSTORM MATERIAL TECH SHANGHAI CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] At present, most of the inorganic layered compounds such as montmorillonite, graphene, and carbon nanotubes are used to prepare flame-retardant nanocomposites. The main flame-retardant effect of these layered nano-composites is sheet barrier effect. to be further improved

Method used

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  • Preparation method of epoxy resin/iron phenyl phosphate composite
  • Preparation method of epoxy resin/iron phenyl phosphate composite
  • Preparation method of epoxy resin/iron phenyl phosphate composite

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Phenylphosphoric acid (Shanghai Sinopharm Chemical Reagent Co., Ltd.), ferric nitrate (Shanghai Sinopharm Chemical Reagent Co., Ltd.), polyvinylpyrrolidone PVP (Shanghai Sinopharm Co., Ltd.) mixed according to the ratio of substances 2:1:0.1:0.3, using ethanol, ethylene glycol and water as solvents, reacted at 170°C for 12 hours, and then dried in an oven at 80°C for 6 hours to obtain FePP nanosheets ; Add 6.8g FePP to acetone and ultrasonically disperse for 20 minutes, then add 121.8g Epoxy L20 and stir and ultrasonically for 30 minutes, remove the acetone under vacuum at 105°C to obtain a viscous mixture. Use a three-roll machine (EXAKT 80E, Germany) to mix this mixture for 30 minutes to obtain a more uniformly dispersed mixture, then preheat it to 125 ° C, add 42.9 g of 4,4'-diaminodiphenylsulfone (DDS) and magnetically stir Mix for 15 minutes to completely dissolve; in order to remove air bubbles, put the mixture in a vacuum oven at 110°C for 5 minutes, then immedia...

Embodiment 2

[0061] The difference from Example 1 is that Epoxy L20, DDS and FePP are evenly mixed according to the mass ratio of epoxy resin (Epoxy L20 and DDS in a mass ratio of 73.7:26.3) and FePP nanosheets to 99:1, and solidified to prepare EP / 1wt% FePP nanocomposite. Compared with pure EP, the flame retardant performance of the obtained composite material is improved, the basic parameters: UL94 test is still not flame retardant grade, but no longer dripping, the oxygen index is increased to 32.5, and the peak heat release rate is reduced to 759kW / m 2 , the total heat release is reduced to 84MJ / m 2 , the peak value of smoke release rate is reduced to 0.1621m 2 / s, the total smoke emission is reduced to 22.9m 2 , the peak CO release rate is reduced to 0.0253g / s, CO 2 The peak release rate decreased to 0.49g / s.

Embodiment 3

[0063] The difference from Example 1 is that Epoxy L20, DDS and FePP are uniformly mixed according to the mass ratio of epoxy resin (Epoxy L20 and DDS in a mass ratio of 73.7:26.3) and FePP nanosheets to 98:2, and solidified to prepare EP / 1wt% FePP nanocomposite. Compared with pure EP, the flame retardant performance of the obtained composite material is improved, and the basic parameters: UL94 test reaches the V-1 flame retardant level, no dripping, the oxygen index is increased to 33.3, and the peak heat release rate is reduced to 691kW / m 2 , the total heat release is reduced to 74MJ / m 2 , the peak value of smoke release rate is reduced to 0.1856m 2 / s, the total smoke emission is reduced to 19.3m 2 , the peak CO release rate is reduced to 0.0202g / s, CO 2 The peak release rate decreased to 0.44g / s.

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Abstract

The invention belongs to the field of new materials and particularly discloses a preparation method of epoxy resin / iron phenyl phosphate composite. The preparation method includes: adding phenyl phosphoric acid, iron nitrate, polyvinylpyrrolidone and hexamethylenetetramine into a mixed solvent of ethanol, ethylene glycol and water to obtain FePP nanosheets; mixing the FePP nanosheets with epoxy resin L20, heating by oil bath, adding a curing agent, dissolving, vacuumizing to remove bubbles, and solidifying in staged manner to obtain epoxy resin / iron phenyl phosphate composite. Combustion performance results show that when the addition of the FePP nanosheets reaches 4% by weight, oxygen index increases to 35.1, reaching V-1 level (t1+t2 equals 15 s), heat release rate peak is 42.6% less than that of pure epoxy resin, and heat release total quantity decreases by about 26.3%; additionally, smoke release total quantity decreases by 32.8%, and CO release quantity decreases by 50.0%. The preparation method herein is simple and feasible, the epoxy resin / iron phenyl phosphate composite has excellent flame retardance and smoke-inhibiting efficiency and is applicable to flame-retardant protection for the matrix materials, such as foam, plastics, and rubber.

Description

technical field [0001] The invention belongs to the field of new materials and relates to a preparation method of epoxy resin / phenyl iron phosphate nanocomposite material. Background technique [0002] Epoxy resin (EP) is a typical thermosetting polymer, which has excellent bonding strength, mechanical properties, electrical insulation and chemical stability, as well as low shrinkage, easy processing and low cost, etc. It has been widely used in high-tech fields such as circuits, transportation, and aerospace [J.Mater.Chem.A, 2015, 3, 6819]. In recent years, the average annual growth rate of epoxy resin is 4.1%. In 2015, the total consumption of epoxy resin in the world reached 2.71 million tons, while the production and sales of epoxy resin in my country accounted for about half of the world's total. However, epoxy resin materials bring fire safety hazards to society due to their flammability. Therefore, in-depth research on high-efficiency flame-retardant epoxy resin com...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L63/00C08K5/53
CPCC08K5/53C08K2201/011C08L2201/02C08L63/00
Inventor 孔庆红孙友亮刘宏陈明毅
Owner TECHSTORM MATERIAL TECH SHANGHAI CO LTD
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