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Preparation method and application of nano composite flame retardant containing DOPO and delamination graphene

A nano-composite and exfoliated graphite technology, applied in the field of flame retardant design, can solve the problems of easy agglomeration and difficulty in dispersion of graphene, and achieve the effect of improving flame retardant performance

Active Publication Date: 2013-05-01
苏州安鸿泰新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the huge specific surface area of ​​graphene and the existence of hydrogen bonds between graphene sheets, graphene is easy to agglomerate.
Therefore, during the preparation of the material, graphene tends to agglomerate, making it difficult to achieve nanoscale dispersion in the polymer matrix.

Method used

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  • Preparation method and application of nano composite flame retardant containing DOPO and delamination graphene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] In a 500 ml three-neck flask equipped with a mechanical stirrer, disperse 1 g of graphene in 200 ml of tetrahydrofuran, stir it ultrasonically to make it evenly dispersed, add 1 g of 3-isocyanatopropyl trimethoxysilane and 0.1 g of dibutyltin dilaurate Ester, heated to 60°C, reacted for 12 hours under continuous stirring, then added 9g of DOPO-VTS-1, 1ml of ammonia water and 9ml of distilled water into the above reaction system, and reacted for 3 hours. The solvent tetrahydrofuran was distilled off under reduced pressure to obtain a black solid powder, which is the nanocomposite flame retardant containing DOPO and exfoliated graphene in this example. The yield was 90%.

[0031] Take 1.25g of the above-prepared black solid powder (i.e. nanocomposite flame retardant containing DOPO and delaminated graphene) and 20g of epoxy resin and stir evenly at 60°C, then add 4.35g of 4,4-diaminodiphenylmethane As a curing agent, pour the flame-retardant epoxy resin liquid into a ...

Embodiment 2

[0033] In a 500 ml three-necked flask equipped with a mechanical stirrer, disperse 1 g of graphene in 200 ml of tetrahydrofuran, stir ultrasonically to make it uniformly dispersed, add 0.3 g of 3-isocyanatopropyltrimethoxysilane and 0.1 g of triethylamine , heated up to 60°C, and reacted for 5 hours under continuous stirring, then added 7g DOPO-VTS-2, 1ml hydrochloric acid, and 9ml distilled water into the above reaction system, and reacted for 3 hours. The solvent tetrahydrofuran was distilled off under reduced pressure to obtain a black solid powder, which is the nanocomposite flame retardant containing DOPO and exfoliated graphene in this example. The yield was 87%.

[0034] Take 1.50g of the black solid powder prepared above (that is, the nanocomposite flame retardant containing DOPO and exfoliated graphene) and 20g of epoxy resin and stir evenly at 60°C, then add 4.35g of 4,4-diaminodiphenylmethane As a curing agent, pour the flame-retardant epoxy resin liquid into a...

Embodiment 3

[0036] In a 500 ml three-neck flask equipped with a mechanical stirrer, disperse 1 g of graphene in 200 ml of chloroform, stir ultrasonically to make it evenly dispersed, add 0.6 g of 3-isocyanatopropyltrimethoxysilane and 0.1 g of dibutyltin di Lauric acid ester, heated up to 70°C, reacted for 12 hours under continuous stirring, then added 8g of the mixture of DOPO-KH-1 and DOPO-KH-2, 1ml of acetic acid, and 8ml of distilled water into the above reaction system, reaction 5 Hour. The solvent chloroform was distilled off under reduced pressure to obtain a black solid powder, which is the nanocomposite flame retardant containing DOPO and exfoliated graphene in this example. The yield was 91%.

[0037] Take 1.75g ​​of the above-prepared black solid powder (i.e. nanocomposite flame retardant containing DOPO and delaminated graphene) and 20g of epoxy resin and stir evenly at 60°C, then add 4.35g of 4,4-diaminodiphenylmethane As a curing agent, pour flame-retardant epoxy resin...

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Abstract

The invention discloses a preparation method and application of a nano composite flame retardant containing DOPO and delamination grapheme. From the angle of improving the dispersity of the graphene, the graphene is modified by silane containing isocyanato, a DOPO structure with efficient fire resistance is introduced through a sol-gel method, and the nano composite flame retardant containing DOPO and delamination graphene is prepared, so that the graphene can form nano-scale delamination dispersion in a polymer, the phosphorus DOPO structure, delamination nanometer dispersion and silicon can achieve synergy, and the flame resistance of the polymer material can be improved remarkably when the retardant is applied in polymer matrixes of epoxy resins, polycarbonate and the like.

Description

[0001] technical field [0002] The invention belongs to the field of flame retardant design, in particular to a method for preparing a nanocomposite flame retardant containing DOPO and exfoliated graphene, and the application of the flame retardant in polymer matrices such as epoxy resin and polycarbonate . Background technique [0003] Due to its rich sources, easy processing, variety, superior performance and low price, polymer materials have been widely used in many fields such as aerospace, electronic information, household appliances, and automobile industry. However, most polymer materials are flammable materials, which are easy to cause fire and cause serious loss of human life and property. Therefore, the flame retardancy of polymer materials is an urgent problem to be solved. 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO) type flame retardant is an organic phosphorus heterocyclic compound. DOPO has high thermal stability, oxidation resistance and exce...

Claims

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Application Information

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IPC IPC(8): C08K9/06C08K3/04C08K5/5435C08L63/00C08L69/00C08L25/06C08L55/02
Inventor 钱晓东时虎
Owner 苏州安鸿泰新材料有限公司
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