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Nano composite material of flame retardant epoxy resin made from salt of phosphate bi melamine

The technology of double melamine salt and nanocomposite is applied in the field of flame retardant epoxy resin material, which can solve problems such as poor flame retardant performance or poor mechanical performance, and achieve the effects of good flame retardancy, environmental friendliness and small addition amount.

Inactive Publication Date: 2007-12-26
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0024] The technical problem to be solved by the present invention is to disclose a phosphate bismelamine salt intumescent flame retardant system and its composite flame retardant epoxy resin with organic montmorillonite to overcome the poor flame retardant or mechanical properties of the prior art. defect

Method used

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  • Nano composite material of flame retardant epoxy resin made from salt of phosphate bi melamine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] In a 500mL three-neck flask, add 15.3mL (0.167mol) POCl 3 , 30g (0.167mol) PEPA, 220mLCH 3 CN, stirred under the protection of nitrogen, and heated until the solids were completely dissolved. Add 12 mL of pyridine dropwise within 5 min, and react for 4 h until the raw material completely disappears. Distillation to remove CH 3 CN, a yellow viscous liquid substance II was obtained. Add 180mL of deionized water, stir for 5h, precipitate a white solid, filter and dry to obtain about 30g, the yield is 70%, and the melting point is about 170°C, which is (1-oxo-4-methylene-2,6,7-tri Oxy-1-phosphabicyclo[2.2.2]octane)phosphate (III).

[0045] In a 500ml three-necked flask, add 22.5g (0.178mol) of melamine and 300ml of deionized water, stir, and heat to reflux. Add 13g (0.050mol) III, reflux for 2h, then add 8.5g (0.033mol) III, reflux for 7h, cool, and precipitate a white solid, filter and dry to obtain 35g of flame retardant (IV), with a yield of 80%. The melting point ...

Embodiment 2

[0047] The amount of raw materials and the operation method are the same as Example 1, the esterification reaction is 7h, III 32g, and the yield is 75%; the salinization reaction is 4h after the first III input; the second III input after the reaction 10h, phosphate bismelamine salt IV 37g , the yield was 85%.

Embodiment 3

[0049] Each stage operation method is identical with embodiment 1. POCl 3 The amount added was 20 mL, and after 4 h of esterification reaction, III was 36 g, and the yield was 83%. At the same time, the first input amount of III was 18 g, and the second input amount was 12 g after 2 hours of reaction. The salinization reaction obtained 40 g of phosphate ester bismelamine salt, and the yield was 92%.

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Abstract

This invention discloses a method for preparing flame-retardant epoxy resin nanocomposite. The method comprises: (1) mixing Na-montmorillonite, organic solvent aqueous solution and silane coupling agent into a reactor, heating to 40-100 deg.C, and reacting for 2-22 h to obtain organic montmorillonite; (2) utilizing 1-oxy-4-hydroxymethyl-2,6,7-trioxy-1-phosphabicyclo[2.2.2]octane, POCl3 and melamine as the raw materials to prepare (1-oxo-4-methylene-2,6,7-trioxy-1-phosphabicyclo[2.2.2]octane)phosphate dimelamine salt flame retardant; (3) adding organic montmorillonite and flame retardant into a mixture of epoxy resin and curing agent m-phenylenediamine, and curing at 80-160 deg.C for 6-12 h to obtain flame-retardant epoxy resin / organic montmorillonite nanocomposite. In the flame-retardant epoxy resin / organic montmorillonite nanocomposite, the flame retardant and organic montmorillonite have good synergistic effect. The flame-retardant epoxy resin nanocomposite has such advantages as low addition amount, good thermal and mechanical properties, and high flame retardancy.

Description

technical field [0001] The invention relates to a flame-retardant epoxy resin material, in particular to a phosphate bismelamine salt flame-retardant epoxy resin nanocomposite material. Background technique [0002] Cured epoxy resin has high mechanical properties, electrical properties and dimensional stability, and is the most widely used matrix resin in polymer materials. In recent years, as people pay more and more attention to the worldwide environmental problems and the safety of human body, the electronics, electrical appliance and coating industries put forward higher requirements on the flame retardant properties of epoxy resins. [0003] In the formulation design of epoxy resin, the application of flame retardants can be divided into two types: additive type and reactive type. Additive flame retardants mainly include phosphate esters (triphenyl phosphate, cresyl diphenyl phosphate, trihalogenated ethyl phosphate, etc.), halogenated organic compounds (chlorinated p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L63/00C08K9/06C08K5/521
Inventor 李到王幸宜胡静平张志慧
Owner EAST CHINA UNIV OF SCI & TECH
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