Preparation method of carbon nanotube amidation grafted polysilsesquioxane flame retardant

A polysilsesquioxane and carbon nanotube technology is applied in the field of preparation of carbon nanotube amidation-grafted polysilsesquioxane flame retardants, which can solve the problem of affecting the mechanical properties of substrates and poor compatibility of substrates. , large amount of flame retardants, etc., to achieve the effect of significant synergy, good compatibility and excellent flame retardant performance

Active Publication Date: 2020-05-19
QUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Halogen-containing flame retardants are gradually eliminated due to the release of toxic gases during thermal decomposition. The above-mentioned patents and prior art halogen-free flame retardants applied to PC mainly include organosilicon, organophosphorus, sulfonate, expansion Type flame retardants, etc. Most of them use condensed phase flame retardant, which has poor compatibility with the substrate. If the addition of flame retardant is too large, it will directly affect the mechanical properties of the substrate.

Method used

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  • Preparation method of carbon nanotube amidation grafted polysilsesquioxane flame retardant
  • Preparation method of carbon nanotube amidation grafted polysilsesquioxane flame retardant
  • Preparation method of carbon nanotube amidation grafted polysilsesquioxane flame retardant

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Effect test

Embodiment 1

[0021] 32 parts of octaaminophenyl silsesquioxanes are added to the reactor, and then under the protection of nitrogen, 1800 parts of surface acyl chloride modified carbon nanotube carbon tetrachloride dispersions with a mass percentage content of 10% are added, 10 parts of biphenyl phosphoramidate, 0.2 parts of aminoferrocene, 3.5 parts of sodium carbonate, stir and mix evenly, reflux reaction for 12 hours, after vacuum distillation, the residue is washed with 25% methanol aqueous solution, and vacuum dried The described carbon nanotube amidation grafted polysilsesquioxane flame retardant is obtained.

[0022] The carbon nanotubes are industrial-grade multi-walled carbon nanotubes with a content of ≥90%.

[0023] The preparation method of the surface acid chloride modified carbon nanotube material is as follows:

[0024] According to the number of parts by mass, 4 parts of carbon nanotubes were added to 100 parts of hydrofluoric acid solution with a mass percentage content o...

Embodiment 2

[0027] 35 parts of octaaminophenyl silsesquioxanes are added to the reactor, and then under the protection of nitrogen, 1900 parts of surface acyl chloride modified carbon nanotube carbon tetrachloride dispersions with a mass percentage content of 12% are added, 12 parts of biphenyl phosphoramidate, 0.8 parts of aminoferrocene, 4.2 parts of sodium carbonate, stir and mix evenly, reflux reaction for 18 hours, after vacuum distillation, the residue is washed with 25% methanol aqueous solution, and vacuum dried The described carbon nanotube amidation grafted polysilsesquioxane flame retardant is obtained.

[0028] The carbon nanotubes are industrial-grade multi-walled carbon nanotubes with a content of ≥90%.

[0029] The preparation method of the surface acid chloride modified carbon nanotube material is as follows:

[0030]According to the number of parts by mass, 8 parts of carbon nanotubes were added to 100 parts of hydrofluoric acid solution with a mass percent content of 15...

Embodiment 3

[0033] 43 parts of octaaminophenyl silsesquioxanes are added to the reactor, and then under the protection of nitrogen, 2400 parts of surface acyl chloride modified carbon nanotube carbon tetrachloride dispersions with a mass percentage content of 15% are added, 15 parts of biphenyl phosphoramidate, 1.5 parts of aminoferrocene, 5 parts of sodium carbonate, stir and mix evenly, reflux reaction for 24 hours, after vacuum distillation, the residue is washed with 25% methanol aqueous solution, and vacuum dried The described carbon nanotube amidation grafted polysilsesquioxane flame retardant is obtained.

[0034] The carbon nanotubes are industrial-grade multi-walled carbon nanotubes with a content of ≥90%. The preparation method of the surface acid chloride modified carbon nanotube material is as follows:

[0035] According to the number of parts by mass, 10 parts of carbon nanotubes were added to 100 parts of hydrofluoric acid solution with a mass percentage content of 20% for ...

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Abstract

The invention relates to the field of preparation of new materials, in particular to a preparation method of a carbon nanotube amidation grafted polysilsesquioxane flame retardant. The preparation method comprises the following steps: surface modification is carried out on a carbon nano tube by adopting tetramethyl guanidino propyl trimethoxy silane; octaaminophenyl silsesquioxane, aminoferroceneand biphenyl phosphoramidate are grafted and introduced into the modified carbon nanotube material by adopting an amidation reaction, and high-heat-resistance and high-smoke-suppression cage-shaped polysilsesquioxane is obtained by virtue of a synergistic effect. The flame retardant has very excellent flame retardance, is used for polycarbonate products, and has the characteristics of small addition amount, strong carbon forming ability and high migration speed.

Description

technical field [0001] The invention relates to the field of material preparation, in particular to a method for preparing a carbon nanotube amidation grafted polysilsesquioxane flame retardant. Background technique [0002] Traditional halogen flame retardants have serious disadvantages such as producing toxic and corrosive fumes, a huge amount of smoke, and serious environmental pollution. Today, with increasingly high requirements for environmental protection and safety, they have long been unable to meet the needs of continuously upgrading material requirements. [0003] CN201711427657.6 discloses a flame retardant, which is composed of the following components in parts by weight: 40-60 parts of ammonium dihydrogen phosphate, 5-10 parts of divinyl triamine, 5 parts of aluminum hydroxide -15 parts, 8-16 parts of magnesium chloride, 10-20 parts of potassium chloride, 5-10 parts of graphite, 10-20 parts of diammonium hydrogen phosphate, and appropriate amount of water. The...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/388C08L69/00C08L83/08
CPCC08G77/045C08L69/00C08L2201/02C08L83/08
Inventor 冯晓亮雷宏赵颖俊吴清盛谢建伟
Owner QUZHOU UNIV
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