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Phosphorus, nitrogen and silicon-containing polymer modified graphene oxide flame retardant and preparation method thereof

A polymer and oxide stone technology, applied in the field of flame retardants, can solve the problem that small molecule modified graphene cannot fully solve the problem of dispersion, and achieve the effects of wide range of use, good flame retardancy and reduced addition amount

Active Publication Date: 2018-07-24
XIAMEN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] CN103073749A discloses a nanocomposite flame retardant containing DOPO and graphene, which uses isocyanate-containing silane to modify graphene, and then grafts DOPO to form a phosphorus-containing, silicon-modified graphene flame retardant , the invention can enhance the flame retardancy of the organic polymer matrix, but the small molecule modified graphene still cannot fully solve the problem of its dispersion in the organic polymer matrix

Method used

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  • Phosphorus, nitrogen and silicon-containing polymer modified graphene oxide flame retardant and preparation method thereof
  • Phosphorus, nitrogen and silicon-containing polymer modified graphene oxide flame retardant and preparation method thereof
  • Phosphorus, nitrogen and silicon-containing polymer modified graphene oxide flame retardant and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] (1) Synthesis of the first polymerized monomer (MAdiDOPO) (reference: CN104262398A).

[0029] (2) Synthesis of the phosphorus-nitrogen-containing silicon polymer (PGMA-co-PMAPOSS-co-PMAdiDOPO):

[0030] First, 2.56g (18mmol) GMA, 16.98g (18mmol) MAPOSS, 22.7g (36mmol) MAdiDOPO (i.e. 1:m:n=10:10:20) and 0.08gAIBN were dissolved in tetrahydrofuran, and after nitrogen gas The oxygen in the solvent was removed by bubbling, and the reaction was carried out at 65°C for 24h. After the reaction, precipitate with methanol for 2 to 3 times to obtain a white powdery solid, which is a silicon-phosphorus-nitrogen-containing polymer.

[0031] (3) Synthesis of the phosphorus-nitrogen-silicon polymer modified graphene oxide flame retardant:

[0032] Get 10g step (2) synthetic phosphorus-nitrogen silicon polymer (PGMA-co-PMAPOSS-co-PMAdiDOPO) 0.1g catalyst tetraoctyl ammonium bromide and 2g graphene oxide are dissolved in N,N-dimethylformamide After 2 hours of ultrasonic dispersion, ...

Embodiment 2～8

[0035] The synthesis operation of the phosphorus-nitrogen-silicon-containing polymer-modified graphene oxide is the same as in Example 1, except that the ratio of different monomers is adjusted by adjusting the value of 1:m:n, that is, the proportion of phosphorus-nitrogen-silicon in the polymer is changed. Specific feed ratios of GMA, MAPOSS, and MAdiDOPO are shown in Table 1:

[0036]

[0037] Table 1

Embodiment 9

[0039] In a three-necked flask equipped with mechanical stirring, add 200 mg of the phosphorus-nitrogen-silicon polymer-modified graphene oxide flame retardant prepared in Example 1 above, then add acetone and ultrasonically disperse it into a black uniform dispersion. Add 7.6 g of E-51 Epoxy resin, after mixing evenly, put it in a vacuum drying oven to remove the solvent, then add 2.2g of DDM curing agent, put it into a self-made polytetrafluoroethylene mold, and put it in an oven for curing. The curing conditions are 120°C for 4 hours, and 140°C for curing 2h, followed by curing at 180°C for 2h to ensure complete curing, and then cooling to room temperature to obtain a flame-retardant epoxy resin material. The product was tested for oxygen index (LOI) according to the method of the national standard GB / T2406.1-2008, and the oxygen index of the material was measured DMA is used to study the dynamic thermomechanical properties of flame-retardant epoxy resin materials. It is mea...

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Abstract

The invention discloses a phosphorus, nitrogen and silicon-containing polymer modified graphene oxide flame retardant and a preparation method thereof. The phosphorus, nitrogen and silicon-containingpolymer modified graphene oxide flame retardant with a good flame retardation property and a good thermal stability is obtained through reasonably adjusting the ratio of MAdiDOPO, MAPOSS and GMA in aphosphorus, nitrogen and silicon-containing polymer and modifying graphene oxide, and the agglomeration problem of graphene and the problem of the dispersibility of the flame retardant in a polymer material are solved.

Description

technical field [0001] The invention belongs to the technical field of flame retardants, and in particular relates to a preparation method of a phosphorus-nitrogen-silicon polymer-modified graphene oxide flame retardant. Background technique [0002] Organic synthetic polymer materials are widely used in electronic devices, aerospace materials, national defense industry, transportation and other fields, but most of these materials are flammable or flammable, which may pose different degrees of fire threats to humans. Traditional halogen-free flame retardant materials mainly add flame retardants containing phosphorus, nitrogen, silicon and other flame retardant elements to the matrix of organic synthetic polymer materials, and achieve the purpose of flame retardant by dissolving or dispersing the flame retardants in the matrix. However, the addition of these flame retardants in large amounts will sacrifice the thermal stability and mechanical properties of the material. [0...

Claims

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Application Information

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IPC IPC(8): C08G83/00C08F230/02C08F230/08C08F220/32C08L87/00C08L63/00
CPCC08F220/32C08F220/325C08F230/02C08G83/001C08L63/00C08L87/005C08F230/08
Inventor 戴李宗李敏王世成洪静刘玲许一婷袁丛辉陈国荣曾碧榕罗伟昂
Owner XIAMEN UNIV
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